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CAS No. : | 4179-19-5 | MDL No. : | MFCD00015435 |
Formula : | C9H12O2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | RIZBLVRXRWHLFA-UHFFFAOYSA-N |
M.W : | 152.19 | Pubchem ID : | 77844 |
Synonyms : |
|
Num. heavy atoms : | 11 |
Num. arom. heavy atoms : | 6 |
Fraction Csp3 : | 0.33 |
Num. rotatable bonds : | 2 |
Num. H-bond acceptors : | 2.0 |
Num. H-bond donors : | 0.0 |
Molar Refractivity : | 44.39 |
TPSA : | 18.46 Ų |
GI absorption : | High |
BBB permeant : | Yes |
P-gp substrate : | No |
CYP1A2 inhibitor : | Yes |
CYP2C19 inhibitor : | No |
CYP2C9 inhibitor : | No |
CYP2D6 inhibitor : | No |
CYP3A4 inhibitor : | No |
Log Kp (skin permeation) : | -5.65 cm/s |
Log Po/w (iLOGP) : | 2.44 |
Log Po/w (XLOGP3) : | 2.23 |
Log Po/w (WLOGP) : | 2.01 |
Log Po/w (MLOGP) : | 1.8 |
Log Po/w (SILICOS-IT) : | 2.29 |
Consensus Log Po/w : | 2.15 |
Lipinski : | 0.0 |
Ghose : | None |
Veber : | 0.0 |
Egan : | 0.0 |
Muegge : | 1.0 |
Bioavailability Score : | 0.55 |
Log S (ESOL) : | -2.46 |
Solubility : | 0.528 mg/ml ; 0.00347 mol/l |
Class : | Soluble |
Log S (Ali) : | -2.25 |
Solubility : | 0.85 mg/ml ; 0.00559 mol/l |
Class : | Soluble |
Log S (SILICOS-IT) : | -3.02 |
Solubility : | 0.144 mg/ml ; 0.000948 mol/l |
Class : | Soluble |
PAINS : | 0.0 alert |
Brenk : | 0.0 alert |
Leadlikeness : | 1.0 |
Synthetic accessibility : | 1.13 |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
43% | Step 1: 4-(2,4-Dimethoxy-6-methyl-phenyl)-4-oxo-butyric acid[0423] To a suspension of l,3-dimethoxy-5-methyl-benzene (5.1O g, 33.55 mmol) and succinic anhydride (3.69 g, 36.91 mmol) in nitrobenzene (100 mL) was added AlCl3 (8.9 g, 67.10 mmol). The reaction mixture was stirred at room temperature for 16 hours then carefully poured into aqueous NaOH. The pH was adjusted to 10 with solid NaOH and the aqueous solution washed with dichloromethane. The pH of the aqueous solution was adjusted to 3 with concentrated HCl and extracted with EtOAc. The organic extracts were dried and concentrated in vacuo. The residue was triturated dichloromethane to give 4-(2,4-dimethoxy-6-methyl-phenyl)-4-oxo-butyric acid as a pale yellow solid (3.7 g, 43%). 1H NMR (400 MHz, MeOD-d4) delta 6.44 (s, IH), 6.40 (s, IH), 3.80 (s, 3H), 3.78 (s, 3H), 3.03 (t, J = 8.1 Hz, 2H), 2.60 (t, J = 8.1 Hz, 2H), 2.19 (s, 3H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
82% | With 2-Iodobenzoic acid; oxone||potassium monopersulfate triple salt; In water; acetonitrile; at 20℃; for 1h; | General procedure: To a suspension of anisole derivative (1.0 mmol), 2-IB (1.0 mmol,248 mg), and Oxone (3.0 mmol, 1.844 g) in MeCN (4 mL) was added water (6 mL). The mixture was stirred at room temperature until complete consumption of the starting material (confirmed by TLCanalysis). Then, the insoluble material was removed by filtration with CH2Cl2 and then the organic layer was extracted with CH2Cl2 (50 mL) at twice. The extract was washed with a saturated NaHCO3 aqueous solution(100 mL) and then filtered through filter paper for dehydration. After the solvent was removed by evaporation, the desired product was purified by flash silica gel chromatography with appropriate solvent. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
72% | With hydrogenchloride; n-butyllithium; In tetrahydrofuran; hexane; | a 2,6-Dimethoxy-4-methylbenzoic acid 104 ml of 1.6M n-butyllithium solution in hexane are added to 200 ml of tetrahydrofuran, followed by dropwise addition of 25 ml of <strong>[4179-19-5]3,5-dimethoxytoluene</strong>, at a temperature between 0 and 5 C. The reaction medium is stirred at 5 C. for 1 h 30, followed by introduction of excess gaseous CO2 over 30 minutes. The mixture is introduced into 200 ml of aqueous 0.5N HCl solution and the aqueous phase is extracted with ethyl acetate. The residue is concentrated and chromatographied on a silica column (eluent: dichloromethane/methanol - 93/7). M.p.=178 C.; Yield: 72%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
74% | With sulfuryl dichloride; In dichloromethane; at 0 - 20℃;Inert atmosphere; | Into a 500-mL 3-necked round-bottom flask, which was purged and maintained with an inert atmosphere of nitrogen, was placed a solution of <strong>[4179-19-5]1,3-dimethoxy-5-methylbenzene</strong> (5 g, 32.85 mmol, 1.00 equiv) in dichloromethane (150 mL). This was followed by the addition of sulfuroyl dichloride (8.869 g, 65.71 mmol, 2.00 equiv) dropwise with stirring at 00 C. Theresulting solution was stirred overnight at room temperature. The pH value of the solution was adjusted to 8 with sodium carbonate (sat. aq.). The resulting solution was extracted with dichloromethane, and the combined organic layers were concentrated under vacuum. The resulting mixture was washed with hexane to give 5.36 g (74%) of 2,4-dichloro-1,5-dimethoxy- 3-methylbenzene as a white solid. |
74% | With sulfuryl dichloride; In dichloromethane; at 0 - 20℃;Inert atmosphere; | Into a 500-mL 3-necked round-bottom flask, which was purged and maintained with an inert atmosphere of nitrogen, was placed a solution of <strong>[4179-19-5]1,3-dimethoxy-5-methylbenzene</strong> (5 g, 32.85 mmol, 1.00 equiv) in dichloromethane (150 mL). This was followed by the addition of sulfuroyl5 dichloride (8.869 g, 65.71 mmol, 2.00 equiv) drop wise with stirring at 0C. The resulting solution was stirred overnight at room temperature. The pH value of the solution was adjusted to 8 with sodium carbonate (sat. aq.). The resulting solution was extracted with dichloromethane, and the combined organic layers were concentrated under vacuum. The resulting mixture was washed with hexane to give 5.36 g (74%) of 2,4-dichloro-1,5-dimethoxy-3-methylbenzene as a white10 solid. |
74% | With sulfuryl dichloride; In dichloromethane; at 0 - 20℃;Inert atmosphere; | Into a 500-mL 3-necked round-bottom flask, which was purged and maintained with an inert atmosphere of nitrogen, was placed a solution of l,3-dimethoxy-5-methylbenzene (5 g, 32.85 mmol, 1.00 equiv) in dichloromethane (150 mL). This was followed by the addition of sulfuroyl dichloride (8.869 g, 65.71 mmol, 2.00 equiv) drop wise with stirring at 0 C. The resulting solution was stirred overnight at room temperature. The pH value of the solution was adjusted to 8 with sodium carbonate (sat. aq.). The resulting solution was extracted with dichloromethane, and the combined organic layers were concentrated under vacuum. The resulting mixture was washed with hexane to give 5.36 g (74%) of 2,4-dichloro-l,5-dimethoxy- 3-methylbenzene as a white solid. |
31 g | With sulfuryl dichloride; In dichloromethane; at 20℃;Cooling with ice; | 1,3-Dimethoxy-5-methylbenzene (30 g, 0.20 mol)And dichloromethane (900 mL) was added to a dry round bottom flask (1 L).Cooling to the above solution in an ice bath sulfuryl chloride (52.5 g, 0.40 mol) was added dropwise.After the dropwise addition was completed, the mixture was stirred at room temperature overnight. After the reaction,Add sodium bicarbonate aqueous sodium hydrogencarbonate solution to adjust pH=8, extract with dichloromethane,Washed with dilute hydrochloric acid, distilled water, and dried,Concentration under reduced pressure gave the compound 2,4-dichloro-1,5-dimethoxy-3-methylbenzene (31 g, white solid). |
31 g | With sulfuryl dichloride; In dichloromethane; at 20℃;Cooling with ice; | <strong>[4179-19-5]1,3-dimethoxy-5-methylbenzene</strong> (30 g, 0.20 mol) and dichloromethane (900 mL) were added to a dry round bottom flask (1 L) and cooled to the above solution in an ice bath. Disulfone chloride (52.5 g, 0.40 mol) was added dropwise, and the mixture was added dropwise and stirred at room temperature overnight. After the reaction was completed, an aqueous solution of sodium hydrogencarbonate was added dropwise to adjust pH = 8, and dichloromethane was extracted with dilute hydrochloric acid, respectively.Washed with distilled water,Drying and concentration under reduced pressure gave compound 2,4-dichloro-1,5-dimethoxy-3-methylbenzene (31 g, white solid). |
31 g | With sulfuryl dichloride; In dichloromethane; at 20℃;Cooling with ice; | <strong>[4179-19-5]1,3-dimethoxy-5-methylbenzene</strong> (30 g, 0.20 mol) and dichloromethane (900 mL) were added to a dry round bottom flask (1 L).To the above solution, a sulfone dichloride (52.5 g, 0.40 mol) was added dropwise under ice-cooling, and the mixture was stirred and stirred at room temperature overnight.After the reaction was completed, NaHCO3 aqueous solution was added dropwise to adjust pH=8, extracted with dichloromethane, washed with dilute hydrochloric acid and distilled water, and dried.Concentration under reduced pressure gave the compound 2,4-dichloro-1,5-dimethoxy-3-methylbenzene (31 g, white solid). |
3.1 g | With sulfuryl dichloride; In dichloromethane; at 20℃;Cooling with ice; | Step 1: Put <strong>[4179-19-5]1,3-dimethoxy-5-methylbenzene</strong> (30g, 0.20mol)And dichloromethane (900 mL) were added to a dry round bottom flask (1 L), and the above solution was added dropwise with dichlorosulfone (52.5 g, 0.40 mol) under ice-cooling,After the addition was complete, the mixture was stirred at room temperature overnight.After completion of the reaction, aqueous NaHCO3 solution was added dropwise to adjust the pH = 8, and dichloromethane was extracted.Wash with dilute hydrochloric acid and distilled water,Dry and concentrate under reduced pressure to obtain compound 2,4-dichloro-1,5-dimethoxy-3-methylbenzene(31g, white solid),Used directly in the next step. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
96% | With dipotassium peroxodisulfate; oxygen; CrH6Mo6O24(3-)*3H3N*3H(1+) In water at 50℃; for 24h; Green chemistry; | |
With potassium permanganate; water |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
91% | With trichlorophosphate; at 0 - 110℃; for 0.75h; | 2No.4-Dimeth.oxy-6-methyl-benzaldehydbeta (4); The Vilsmeier reagent was prepared by the drop wise addition over 15 min of phosphoryl chloride (5.6ialphaL, 1.2eq) to a stirred solution of dry DMF (1OmL) under nitrogen at 00C. The mixture was allowed to warm to room temperature and was then added over a period of -30 min to a stirred solution of 2,4-dimethoxy-6-methylbenzene (50mmol, 7.betag, 1. Oeq) in 15mL of dry DMF at 100-1103C oil bath, under nitrogen atmosphere. Heating and stirring were continued until TLC indicated that the substrate lias been consumed (~lh) . The mixture was poured onto ice-water, made slightly basic (pH~8) i>Upsilon the addition of aqueous saturated solution of K2CO3. The purple soliition became yellow and the solid precipitate formed was isolated and dried in a dessicator over -P2O5 to afford 8.2g (91%) of 2,4-dimethoxy-6-methyl- benzaldehycle (4) as an off-white solid.1H NMR (CDCl3) 400MHz deltaltheta.47 (IH, s) , 6.32 (2H, s) , 3.87 (3H, s), 3.85 (3H, s), 2.58 (3H, s).13C NMR (CDCl3) 100MHz 6190.5, 165.1, 164.5, 144.7, 117.3, 108.8, 95.7, 55.7, 55.4, 22.3. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1.1: O3 / CH2Cl2; methanol / -78 °C 1.2: 60 percent / Ph3P / CH2Cl2; methanol / 0.5 h 2.1: 87 percent / H2 / 10 percent Pd/C / ethanol / 20 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
88% | 231.6 g (1.5 mol) of <strong>[4179-19-5]3,5-dimethoxytoluene</strong> are dissolved in 1 litre of diethylether, followed by dropwise addition, under nitrogen and at room temperature, of 1 litre of a 1.6 N solution of butyllithium (1.6 mol) in hexane. The reaction mixture is left for 18 hours at room temperature and then, after cooling to 30 C., 1 litre of diethylether is added and carbon dioxide is bubbled through for one hour, while maintaining the temperature at 30 C. The reaction mixture is taken up in 6 litres of 2 M sodium hydroxide solution, the aqueous phase is separated out after settling has taken place and is acidied with 6 N hydrochloric acid solution. The precipitate formed is ltered off, rinsed with water and dried under vacuum at 40 C. in order to obtain white crystals; m.p.=187 C.; yield=88%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
82% | With potassium carbonate; dimethyl sulfate; In acetonitrile; | Example 44 (Reference Example) 3,5-dimethoxy toluene Commercially available orcinol (5.77 g) was dissolved in acetonitrile (200 ml), dimethyl sulfate (8.47 ml) and potassium carbonate (12.3 g) were added, and the admixture was refluxed for 2.5 hours. The reaction mixture was poured into ice water and partitioned with chloroform, and the chloroform layer was dried with anhydrous magnesium sulfate. The solvent was removed by reduced-pressure distillation, and the resulting residue was purified by column chromatography on silica gel eluding with hexane/ethyl acetate (5/1) to obtain 5.04 g of the title compound (yield: 82%). 1 H-NMR (CDCl3, 500 MHz): delta 2.30 (s, 3H), 3.76 (s, 6H), 6.30 (s, 1H), 6.37 (s, 2H) |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
80% | With hydrogenchloride; n-butyllithium; In diethyl ether; hexane; | Stage 1 300 ml of a solution (1.6M) of butyllithium in hexane are added dropwise at room temperature to a solution of 73 g of <strong>[4179-19-5]3,5-dimethoxytoluene</strong> in 450 ml of diethyl ether. The reaction mixture is heated at reflux for 3 hours under an inert atmosphere, the reaction mixture is then cooled to -60 C. and 99.7 g of methyl borate are added dropwise over 60 minutes. The reaction mixture is left at -60 C. for 3 hours and left to return to room temperature. The reaction mixture is stirred at room temperature for 16 hours, 6N hydrochloric acid is then added to the reaction mixture (pH=1) and the reaction mixture is left to separate by settling. The organic phase is recovered. The aqueous phase is extracted with diethyl ether. The combined organic phases are dried over anhydrous sodium sulphate. Evaporation of the solvent leaves a yellow oil which crystallizes by cooling to 0 C. After drying, white crystals of 2,6-dimethoxy-4-methylphenylboronic acid are recovered, M.p.=108 C., Yield 80%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
66% | With chlorosulfonic acid; sodium hydroxide; carbonic acid dimethyl ester; In cyclohexane; at 20 - 72℃; for 1.25h; | To a 3-necked, round-bottomed flask was added <strong>[4179-19-5]3,5-dimethoxytoluene</strong> (6.088 g, 40 mmol) and cyclohexane (28 mL) under nitrogen. Dimethyl carbonate (30.3 g, 336 mmol) was added and the reaction mixture was heated at 60 C. Excess chlorosulfonic acid was added over a period of 15 min. The liberated HCl gas was removed by inserting a tube into solid sodium hydroxide. On completion of the addition, the reaction mixture was heated to 70-72 C. for 1 h and then cooled to room temperature. The solid was filtered off and washed with dimethyl carbonate/cyclohexane (1:1, 20 mL). The solid was dried in vacuo to obtain pure material (6.13 g, 66%). To a mixture of the sulfonic acid (product from above, 4.65 g, 20 mmol) and triethyl amine (2.03 g, 2.79 mL) in acetone (40 mL) was added 2,4,6-trichloro-1,3,5-triazine (cyanuric chloride, 3.69 g, 20 mmol). The reaction mixture was heated under reflux for 20 h before being cooled to room temperature. The solution was passed through a Celite pad and evaporated in vacuo to leave a solid, which was filtered off and washed with hexane. The mixture of product and salt of cyanuric hydroxide and triethyl amine (7.58 g) was used for the next step without further purification.To a 3-necked, round-bottomed flask, equipped with a condenser (acetone-dry ice cooling), was added the mixture from the step above (7.58 g) and acetone (100 mL). The reaction mixture was cooled to -78 C. and ammonia gas was bubbled through the solution for 0.5 h. The reaction mixture was kept standing overnight, allowing slow evaporation of ammonia gas, followed by the evaporation of solvent. Water was added and the product was extracted with DCM. The solvent was dried and evaporated to leave a mixture of solid and a dense liquid. The solid was filtered off and washed with hexane to leave pure sulfonamide (3.23 g, 70%).To a round-bottomed flask was added 3,5-dimethyl-4-hydroxybenzoic acid (2.99 g, 18 mmol). Anhydrous DMF (20 mL) was added, followed by sodium hydride (1.8 g, 45 mmol). The reaction mixture was stirred at room temperature for 1 h. p-Methoxybenzyl chloride (6.20 g, 39.6 mmol) was added and the mixture was stirred at room temperature overnight (20 h). The reaction mixture was poured into water, acidified with 1 N HCl and stirred for 1 h. The precipitated solid was filtered off, washed with water and hexane to obtain pure B-ring building block (6.93 g, 95%).The B-ring building block (6.93 g, 17.1 mmol) was dissolved in a mixture of methanol (50 mL) and tetrahydrofuran (50 mL). Potassium hydroxide (1.25 g, 22.2 mmol) in water (20 mL) was added. The reaction mixture was refluxed at 70 C. for 24 h. The solvent was evaporated in vacuo. Water was added and the reaction mixture was acidified with 1 N HCl (pH 4-5). The solid was filtered off, washed with water and hexane. The yield was 4.61 g (94%). The product (1.932 g, 6.75 mmol) and the sulfonamide from above (1.04 g, 4.5 mmol) were taken in a 3-necked, round-bottomed flask under nitrogen. Dichloromethane (100 mL) was added with stirring. To this stirred mixture was added N-(3-dimethylaminopropyl)-N'-ethylcarbodiimide hydrochloride (EDCl. HCl, 1.36 g, 7.09 mmol), followed by N,N-dimethylaminopyridine (2.06 g, 16.9 mmol). The reaction mixture was stirred at room temperature for 24 h before being washed with 1 N HCl, 2.5% NaOH and saturated sodium bicarbonate solutions. The organic layers were dried and evaporated in vacuo to leave a residue, which was purified by silica gel (100 g) column chromatography, employing 20-50% ethyl acetate in hexane and 5% methanol in dichloromethane as eluents. Fractions 30-66 were combined to obtain pure materials (1.35 g, 60%). The compound from the step above (0.105 g, 0.21 mmol) was dissolved in tetrahydrofuran under nitrogen and cooled to -78 C. n-Butyllithium was added and the reaction mixture was allowed to warm to room temperature slowly and stirred overnight (14 h). TLC showed incomplete conversion. The reaction mixture was quenched with saturated ammonium chloride solution and extracted with ethyl acetate. The solvent was evaporated in vacuo to leave a residue that was purified by silica gel (15 g) column chromatography, employing 20-50% ethyl acetate in hexane as eluents. The product was not pure enough, so another column was used, employing 0.5% methanol in hexane as eluent, and finally preparative TLC was employed to purify the material. The compound from the step above (0.277 g) was dissolved in trifluoroacetic acid (10 mL) under nitrogen and the reaction mixture was refluxed (bath temperature 80 C.) for 4 d. The solvent was evaporated in vacuo and the residue was dissolved in 0.25 N NaOH (20 mL), and acidified with acetic acid. The solid had precipitated out at this point. The solid was filtered off and washed with water, hexane and dried. From one batch, 0.005 g of pure material was isolated. From another batch, 0.060 g compound was isolated, which was not pure enough. This compound was further purified by preparat... |
66% | A 3-necked round bottom flask was added <strong>[4179-19-5]3,5-dimethoxytoluene</strong> (6.088g, 40mmol) and cyclohexane(28mL) under nitrogen.Was added dimethyl carbonate (30.3g,336mmol), at 60 deg.] Cand the reaction mixture was heated. After 15 minutes was added an excess of chlorosulfonic acid. By inserting the tubeof solid sodium hydroxide to remove HCl gas release. After the addition wascomplete, the reaction mixture was heated at 70-72 for one hour, then cooled toroom temperature. The solid was filtered off, washed with dimethyl carbonate /cyclohexane (1:1,20mL)and washed. The solid was dried under vacuum to give pure material (6.13g, 66%). To sulfonic acid (product fromthe above, 4.65g, 20mmol) and triethylamine(2.03g, 2.79mL) was added 2,4,6-trichloro-1,3,5triazine (cyanuric chloride, 3.69g, 20mmol)in (40 mL) in amixture of acetone-.The reaction mixture was heated at reflux for 20 hours, then cooled to room temperature. Thesolution was passed through a pad of Celite, and evaporated in vacuo to leave asolid, which was filtered off, washed with hexane. The product of cyanuric acidand hydroxides (cyanuric hydroxide) in a mixture of salt and triethylamine (was7.58 g) used in the next step without further purification. Fitted to acondenser (acetone - cooled with dry ice), 3-neck round bottom flask was addedthe mixture from step (was 7.58 g) and acetone (100mL). Thereaction mixture was cooled to -78 , ammonia gas intothe solution for 0.5hours. The reaction mixture was allowed to stand overnight, so that theammonia was slowlyevaporated, and then the solvent was evaporated. Water was added, the productwas extracted with DCM. The solvent was dried and evaporated to a mixture ofthe remaining solid and thick liquids. The solid was filtered off, washed withhexane, the remaining pure sulfonamide (3.23g,70%). To a round bottomflask was added 3,5-dimethyl-4-hydroxybenzoicacid (2.99g, 18mmol). Was added anhydrous DMF (20mL), and sodium hydride (1.8g, 45mmol). The reaction mixturewas stirred at roomtemperature for 1hour. Was added p-methoxybenzyl chloride (6.20g,39.6mmol), and the mixture was stirred at room temperature overnight (20 hours). Thereaction mixture was poured into water, acidified with 1N HCl and stirred for 1hour. The precipitated solid was filtered off, washed with water and hexane togive the pure B- cyclic structural unit (6.93g, 95%). The structural unitof the B- ring (6.93g, 17.1mmol) was dissolvedin a mixture of methanol(50mL) and tetrahydrofuran(50 mL) of. Waterwas added (20 mL) of potassium hydroxide (1.25g,22.2mmol). At 70 deg.] Cand the reaction mixture was refluxed for 24 hours. The solvent was evaporated in vacuo.Water was added, the reaction mixture was acidified with 1N HCl (pH4-5). Thesolid was filtered off, washed with water and hexanes. The yield was 4.61g (94%). Under nitrogen,above product (1.932g, 6.75mmol), and sulfonamidefrom above (1.04g, 4.5mmol) was added to a 3-neck round bottom flask. Dichloromethane was addedunder stirring (100mL). To this stirred mixture was addedN-(3-dimethylaminopropyl)-N'-ethylcarbodiimide hydrochloride (EDCI.HCl, 1.36g, 7.09mmol), followed by addition of N, N- dimethylaminopyridine(2.06g, 16.9mmol). At roomtemperature the reaction mixture was stirred for 24 hours, then washed with 1N HCI, 2.5%NaOH and saturated sodium bicarbonate solution. The organic layer was dried andevaporated in vacuo to leave a residue, which was purified by silica gel (100g)column chromatography using 20-50% hexane in ethyl acetate in methylenechloride and methanol as the eluting 5% purification agent. Fractions 30-66afforded pure material (1.35g, 60%). Under nitrogen,compounds from the previous step(0.105g, 0.21mmol) was dissolved in tetrahydrofuran, cooled to -78 . N-butyllithium was added, and the reaction mixture wasslowly warmed to roomtemperature and stirredovernight (~ 14 hours).TLC showed incomplete conversion. The reaction mixture was quenched withsaturated ammonium chloride solution, extracted with ethyl acetate. The solventwas evaporated in vacuo, the remaining residue, which was purified by silicagel (15g) column chromatography adopt in 20-50% ethyl acetate in hexanes aseluent. Product was not pure enough, thus making use of another pillar, the useof hexane in 0.5% methanol as eluent. Finally, the material was purified bypreparative TLC. Under nitrogen compounds from the previous step(0.277 g of) was dissolved in trifluoroacetic acid (10mL), and the reaction mixture was refluxed (bath temperature 80 ) 4 days. The solvent wasevaporated in vacuo, the residue was dissolvedin 0.25N NaOH (20mL), and acidified with acetic acid. At this time, the solidhas precipitated. The solid was filtered off, washed with water, washed withhexane, and dried. 0.005g of pure substances isolated from the batch. 0.060gcompound isolated from another batch, which is not enough pure. The compoundwas further purified by preparative HPLC, to give pure 6,8-dimethoxy-3-(4-hydroxy-3,5-dimethylphenyl) -2H-1,2- benzothiazine 1,1-... | |
66% | With chlorosulfonic acid; carbonic acid dimethyl ester; In cyclohexane; at 60 - 72℃; for 1.25h; | To a 3-necked, round-bottomed flask was added 3,5- dimbetathoxytoluene (6.088 g, 40 mmol) and cyclohexane (28 mL) under nitrogen. Dimethyl carbonate (30.3 g, 336 mmol) was added and the reaction mixture was heated at 60C. Excess chlorosulfonic acid was added over a period of 15 min. The liberated HCI gas was removed by inserting a tube into solid sodium hydroxide. On completion of the addition, the reaction mixture was heated to 70-72C for 1 h and then cooled to room temperature. The solid was filtered off and washed with dimethyl carbonate/cyclohexane (1:1, 20 mL). The solid was dried in vacuo to obtain pure material (6.13 g, 66%). To a mixture of the sulfonic acid (product from above, 4.65 g, 20 mmol) and tribetathyl amine (2.03 g, 2.79 mL) in acetone (40 mL) was added 2,4,6-trichloro-i ,3,5-triazine (cyanuric chloride, 3.69 g, 20 mmol). The reaction mixture was heated under reflux for 20 h before being cooled to room temperature. The solution was passed through a Celite pad and evaporated in vacuo to leave a solid, which was filtered off and washed with hexane. The mixture of product and salt of cyanuric hydroxide and triethyl amine (7.58 g) was used for the next step without further purification.[0156] To a 3-necked, round-bottomed flask, equipped with a condenser (acetone-dry ice cooling), was added the mixture from the step above (7.58 g) and acetone (100 mL). The reaction mixture was cooled to -78C and ammonia gas <n="93"/>was bubbled through the solution for 0.5 h. The reaction mixture was kept standing overnight, allowing slow evaporation of ammonia gas, followed by the evaporation of solvent. Water was added and the product was extracted with DCM. The solvent was dried and evaporated to leave a mixture of solid and a dense liquid. The solid was filtered off and washed with hexane to leave pure sulfonamide (3.23 g, 70%).[0157] To a round-bottomed flask was added 3.5-dimethyl-4- hydroxybenzoic acid (2.99 g. 18 mmol). Anhydrous DMF (20 rnL) was added, followed by sodium hydride (1.8 g, 45 mmol). The reaction mixture was stirred at room temperature for 1 h. p-Methoxybenzyl chloride (6.20 g, 39.6 mmol) was added and the mixture was stirred at room temperature overnight (-20 h). The reaction mixture was poured into water, acidified with 1 N HCI and stirred for 1 h. The precipitated solid was filtered off, washed with water and hexane to obtain pure B-ring building block (6.93 g, 95%).[0158] The B-ring building block (6.93 g, 17.1 mmol) was dissolved in a mixture of methanol (50 ml) and tetrahydrofuran (50 mL). Potassium hydroxide (1.25 g, 22.2 mmol) in water (20 mL) was added. The reaction mixture was refluxed at 709C for 24 h. The solvent was evaporated in vacuo. Water was added and the reaction mixture was acidified with 1 N HCI (pH 4-5). The solid was filtered off, washed with water and hexane. The yield was 4.61 g (94%). The product (1.932 g, 6.75 mmol) and the sulfonamide from above (1,04 g, 4.5 mmol) were taken in a 3-necked, round-bottomed flask under nitrogen. Dichloromethane (100 mL) was added with stirring. To this stirred mixture was added N-(3- dimethylaminopropyl)-W-ethylcarbOdiimide hydrochloride (EDCI. HCI, 1.36 g,7.09 mmol), followed by lambda/,W-dimethylaminopyridine (2.06 g, 16.9 mmol). The <n="94"/>reaction mixture was stirred at room temperature for 24 h before being washed with 1 N HCI, 2.5% NaOH and saturated sodium bicarbonate solutions. The organic layers were dried and evaporated in vacuo to leave a residue, which was purified by silica gel (100 g) column chromatography, employing 20-50% ethyl acetate in hexane and 5% methanol in dichloromethane as eluents. Fractions 30-66 were combined to obtain pure materials (1.35 g, 60%). The compound from the step above (0.105 g, 0.21 mmol) was dissolved in tetrahydrofuran under nitrogen and cooled to -78C. n-Butyllithium was added and the reaction mixture was allowed to warm to room temperature slowly and stirred overnight (~14 h). TLC showed incomplete conversion. The reaction mixture was quenched with saturated ammonium chloride solution and extracted with ethyl acetate. The solvent was evaporated in vacuo to leave a residue that was purified by silica gel (15 g) column chromatography, employing 20-50% ethyl acetate in hexane as eluents. The product was not pure enough, so another column was used, employing 0.5% methanol in hexane as eluent, and finally preparative TLC was employed to purify the material. The compound from the step above (0.277 g) was dissolved in trifiuoroacetic acid (10 mL) under nitrogen and the reaction mixture was refluxed (bath temperature 809C) for 4 d. The solvent was evaporated in vacuo and the residue was dissolved in 0.25 N NaOH (20 mL), and acidified with acetic acid. The solid had precipitated out at this point. The solid was filtered off and washed with water, hexane and dried. From one batch, 0.005 g of pure material was isolated. From another batch, 0.060 g compound was isolated, which was not pure enough... |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
81% | 3,5-Dimethoxytoluene (2.93 ml_, 20 mmol) and 4-phenylbutylbromide (4.13 ml_, 1.2 mmol) were reacted as described under General Procedure H and the crude product was purified by flash chromatography (silica-gel, petroleum ether/EtOAc 200:1) to afford the product as a clear oil (4.6 g, 81%). 1H NMR (300 MHz, CDCI3) delta 7.13-7.22 (m, 5H), 6.34 (s, 2H), 3.76 (s, 6H), 2.60-2.64 (m, 4H), 2.31 (s, 3H), 1.53-1.67 (m, 4H).; General Procedure H: Alkylation of <strong>[4179-19-5]3,5-dimethoxytoluene</strong> A solution of n-butyllithium in hexanes (1.7 M, 1.2 eq.) was added over 0.25 h to a solution of <strong>[4179-19-5]3,5-dimethoxytoluene</strong> (1.0 eq.) in THF (1 M) at 0 0C. The reaction mixture was stirred at 0 0C for 1 h then at room temperature for 3 h. The reaction was cooled to 0 0C and a solution of the alkyl bromide (1.2 eq.) in toluene (2 M) was added over 0.1 h. The reaction mixture was allowed to warm to room temperature and heated to 80 0C for 3-4 h. The reaction was quenched slowly with water and partitioned over EtOAc and water. The phases were separated and the <n="47"/>aqueous phase was extracted twice with EtOAc. The pooled organics were washed with brine, dried over Na2SO4 and concentrated under vacuum. The residue was purified by flash chromatography. | |
81% | 68a) 1,3-Dimethoxy-5-methyl-2-(4-phenylbutyl)benzene; :A solution of nBuLi in hexanes (1.7 M, 14 ml_, 24 mmol) was added over 15 min to a solution of <strong>[4179-19-5]3,5-dimethoxytoluene</strong> (2.93 ml_, 20 mmol) in THF (20 mL) at 0 0C. <n="115"/>The reaction mixture was stirred at 0 C for 1 h then at room temperature for 3 h. The reaction was cooled to 0 0C and a solution of the 4-phenylbutylbromide (4.13 ml_, 1.2 mmol) in toluene (15 mL) was added over 5 min. The reaction mixture was allowed to warm to room temperature and heated to 80 0C for 3-4 h. The reaction was quenched slowly with water and partitioned over Et2theta (100 mL) and water (100 mL). The phases were separated and the aqueous phase was extracted with Et2O (3 x 100 mL). The pooled organics were washed with brine (120 mL), dried over Na2SO4, and concentrated under vacuum and the crude product was purified by flash chromatography (silica-gel, petroleum ether / EtOAc 200:1) to afford the product as a clear oil (4.6 g, 81 %). 1H NMR (CDCI3): delta 1.53-1.67 (m, 4H), 2.31 (s, 3H), 2.60-2.64 (m, 4H), 3.76 (s, 6H), 6.34 (s, 2H), 7.13-7.22 (m, 5H)1. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
98% | With trifluoroacetic acid; In dichloromethane; at 20℃; for 0.0166667h; | a All reactions were conducted according to a standard procedure unless otherwise specified: MeTAD (1 mmol) was added to a stirring solution of the substituted benzene (1.5 mmol) in 10 mL of solvent. The acid catalyst (equivalents provided in the Table) was added via syringe. If the reaction required heating, the solution was heated at reflux with a drying tube attached to the reflux condenser. Upon completion of the reaction, the solvent was removed via rotary evaporation. The resulting reaction mixture was subjected to column chromatography on SiO2 using ethyl acetate as eluent. Characterization information for all new compounds is provided in Supplementary data.b UH = N-4-methylurazole with N-1 attached to the aromatic ring and N-2 attached to an H.c A 19% yield of compounds 4 and 5 (in a 60:40 ratio) was also isolated. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
78% | Stage #1: 1,3-dimethoxy-5-methylbenzene With n-butyllithium In tetrahydrofuran Stage #2: methyl iodide | |
73% | Stage #1: 1,3-dimethoxy-5-methylbenzene With 2,2,6,6-tetramethyl-piperidine; n-butyllithium; potassium <i>tert</i>-butylate In tetrahydrofuran at -78℃; for 1h; Inert atmosphere; Stage #2: methyl iodide In tetrahydrofuran at -78℃; for 0.5h; Inert atmosphere; regioselective reaction; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
79% | With N1,N1,N12,N12-tetramethyl-7,8-dihydro-6H-dipyrido[1,2-a:2,1'-c][1,4]diazepine-2,12-diamine In N,N-dimethyl-formamide at 20℃; for 72h; Glovebox; UV-irradiation; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
82% | With dimethylsulfoxide-d6; potassium tert-butylate; at 80℃; for 1h;Inert atmosphere; | General procedure: To a solution of KOt-Bu (11.3 mg, 0.1 mmol) in DMSO-d6 (1.5 mL) was added N,N-dimethyl-1-phenylmethanamine (135.0 mg,1.0 mmol). The reaction mixture was then stirred at 80 C under argon atmosphere for 1.0 h. After being cooled to room temperature,the reaction mixture was poured into water (10 mL), and followed by the extraction with ethyl acetate (15 mL3). The combined organic layer was dried over anhydrous MgSO4 and concentrated under vacuum. The residue was purified by flash column chromatography over silica gel to give 2a as a colorless oil (119.0 mg, 87% yield). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
21% | General procedure: A 0.94 M soln of MeMgBr in THF (1.59 mL, 1.5 mmol) was added to a mixture of FeF3 (5.7 mg, 0.050 mmol) and 1,3-bis(2,6-diisopropylphenyl)imidazolinium chloride (64.4 mg, 0.15 mmol) in THF (2.0 mL) at 0C; 1-chloro-4-methoxybenzene (143 mg, 1.0 mmol) and undecane were then added at r.t. The mixture was stirred at 80 C for 24 h. The mixture was cooled to r.t. and an aliquot of the mixture was filtered through a Florisil pad. The product yield was determined by GC analysis (92% yield) using undecane as an internal standard. 1-Methoxy-4-methylbenzene is volatile, hence isolation was performed for the large-scale experiment using starting aryl chloride (5.6 mmol). The crude product was purified by column chromatography (silica gel, pentane, Rf = 0.06) and subsequent GPC to obtain the title compound (78.7 mg, 11%) as a colorless oil. | |
21% | General procedure: A THF solution of methyl magnesium bromide (1.59 mL, 0.94 M, 1.5 mmol) was added to a mixtureof FeF3 (5.7 mg, 0.050 mmol) and1,3-bis(2,6-diisopropylphenyl)imidazolinium chloride (64.4 mg, 0.15 mmol) in2.0 mL of THF at 0 C. The substrate aryl chloride, 1-chloro-4-methoxybenzene (143 mg, 1.0 mmol), and undecane werethen added at room temperature. The mixture was stirred at 80 C for 24 h.After cooling to room temperature, an aliquot of the reaction mixture was filtered through a Florisil pad. The product yield was determined by GC analysis (92% yield) using undecane as an internal standard. To avoid loss ofproducts, isolation was performed in the large-scale experiment using 5.6 mmolof the starting aryl chloride. After the reaction was performed at 80 C for 84 h, saturated aqueous sodium potassium tartrate and aqueous HCl (1 N) wereadded. The aqueous layer was extracted with ether four times. The organic layerwas combined, washed with brine, dried over Na2SO4, andfiltered through a Florisil pad. After removal of the solvent, the crudeproduct was purified by silica gel column chromatography using pentane as theeluent (Rf = 0.06) and subsequent GPC to obtain the title compound (78.7 mg, 11%) as a colorless oil. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
34% | With Selectfluor; In acetonitrile; at 0 - 20℃; | To a solution of <strong>[4179-19-5]1,3-dimethoxy-5-methylbenzene</strong> (4 g, 26.28 mmol) in ACN (60 mL) at 0C was added Selectfluor (8.4 g, 23.73 mmol) drop wise with stirring. The resulting solution was stirred overnight at room temperature and then quenched with water. The resulting solution was extracted with DCM and the organic layers combined and concentrated. The residue was purified by chromatography (ethyl acetate/pet. ether (1:20)) to afford 1.5 g (34%) of 2-fluoro- 1,5-dimethoxy-3-methylbenzene as colorless oil. |
34% | With Selectfluor; In acetonitrile; at 0 - 20℃; | To a solution of l,3-dimethoxy-5-methylbenzene (4 g, 26.28 mmol) in ACN (60 mL) at 0 C was added Selectfluor (8.4 g, 23.73 mmol) drop wise with stirring. The resulting solution was stirred overnight at room temperature and then quenched with water. The resulting solution was extracted with DCM and the organic layers combined and concentrated. The residue was purified by chromatography (ethyl acetate/pet. ether (1 :20)) to afford 1.5 g (34%) of 2-fluoro- l,5-dimethoxy-3-methylbenzene as colorless oil. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
49% | With sodium tetrafluoroborate; potassium iodide; In acetonitrile; at 60℃; for 6h;Electrochemical reaction; | Electrolysis experiments were performed on Vertex Potentiostat/Galvanostat. Both the working electrode and the counter electrode were made of platinum (1.5cm×1.5cm). Ag/Ag+ electrode (0.1mol/L AgNO3 in CH3CN) was employed as the reference electrode. The 0.1mol/L of NaBF4/CH3CN solution (15mL) with 1,3,5-trimethoxybenzene (1a, 0.5mmol, 84mg), 4-chlorothiophenol (2a, 0.6mmol, 86mg) and KI (0.05mmol, 8.3mg) was added into a 25mL undivided beaker and the resulting mixture was stirred at 60C. After completion of the reaction (analysed by GC or TLC), the resulting mixture was concentrated under reduced pressure and purified by column chromatography on 200-300 mesh silica gel using petroleum ether: ethyl acetate (50:1) as eluent to afford (4-chlorophenyl) (2,4,6-trimethoxyphenyl)sulfane (3aa) as a white solid in 90% yield. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
95% | With nickel-doped graphene carbon nitride nanoparticles; air In ethanol at 25℃; for 8h; Irradiation; Green chemistry; | General procedure for C-H activation reactions General procedure: A mixture of toluene (1 mmol) in EtOH (2 mL)) placed in 10 mL round bottom flask, nano Ni/g-C3N4 (6 wt%, 0.01 g) was added and the reaction was irradiated by 12 W blue LED Lamp (λ > 440 nm, distance app. 4.0 cm) in open-air condition. The reaction was stirred for the appropriate time at room temperature (25 °C) and monitored by TLC. After completion, the reaction mixture was centrifuged to separate the photocatalyst, then, the reaction was diluted with ethyl acetate (12mL) and final product purification was done through silica gel column chromatography using petroleum ether/ethyl acetate. |
Multi-step reaction with 2 steps 1: N-Bromosuccinimide / acetonitrile / 1 h / 25 °C / Inert atmosphere 2: hexamethylenetetramine / water / 12 h / 120 °C / Inert atmosphere |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
88% | With hydrogenchloride; In water; at 120℃; for 6h; | 5 mg of 3,5-trimethoxytoluene (76 mg), 1,3-dimethoxybenzene (69 mg) or 1,3-bisEthoxybenzene (83 · lmg), 0.75 mmol of sodium p-methoxybenzenesulfinate (145.6 mg), and 1.2 mmol of hydrochloric acid (36.5% of hydrochloric acid, 102.6 mil) were added to a pressure- 0.5 mL of ionic liquid was reacted at 120 C for 6 h. After the reaction was complete, the mixture was extracted three times with 2 mL of ethyl acetate. The organic solvent was removed by steaming and passed through a column of silica gel to give the target product 4a-4c in 88% yield, 86%, 91%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 10 steps 1: sulfuryl dichloride / dichloromethane 2: N-Bromosuccinimide; 2,2'-azobis(isobutyronitrile) / tetrachloromethane 3: dimethyl sulfoxide 4: potassium carbonate / N,N-dimethyl-formamide / 100 °C 5: sodium nitrite; acetic acid 6: potassium carbonate / acetone / Reflux 7: 3-chloro-benzenecarboperoxoic acid / chloroform 8: tetrahydrofuran; <i>tert</i>-butyl alcohol / 60 °C 9: hydrogenchloride / 1,4-dioxane 10: triethylamine / dichloromethane |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
65% | With N-hydroxyphthalimide; oxygen; tetra-(n-butyl)ammonium iodide; In acetonitrile; at 75℃; | General procedure: A 50 mL three-necked round bottom flask equipped with a magnetic stir bar was charged with toluene derivatives2 (3.0 mmol), olefin (1.0 mmol), NHPI (16.3 mg, 10 mol %), Bu4NI (36.9 mg, 10 mol %) in MeCN (8.0 mL) at roomtemperature. O2 was bubbled into the mixture at 75 C for 6-12 hours. After the reaction was completed, it wasmonitored by TLC. The resulting solution was poured into NaCl (15 mL), extracted with DCM (twice). The combinedorganic layers were dried over anhydrous Na2SO4 and solvents were removed in vacuo. The residue was purified byPLC- Silica Gel Plate (eluant: petroleum ether/ethyl acetate = 30:1) to give the desired product. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
67% | With toluene-4-sulfonic acid; In acetonitrile; at 80℃; for 3h; | General procedure: A 25mL round-bottom flask equipped with a magnetic barand a water condenser was charged with propargylic alcohol1 (1.0mmol), arene 2 (1.1mmol), MeCN (2.0mL) andPTSA (10mol%) in air atmosphere. The flask was placedinto a constant temperature oil-bath at 80C and the progressof the reaction was monitored by TLC. After completionof the reaction, the solvent was removed under reducedpressure and the crude reaction mixture was purified by columnchromatography. |
Tags: 4179-19-5 synthesis path| 4179-19-5 SDS| 4179-19-5 COA| 4179-19-5 purity| 4179-19-5 application| 4179-19-5 NMR| 4179-19-5 COA| 4179-19-5 structure
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H340 | May cause genetic defects |
H341 | Suspected of causing genetic defects |
H350 | May cause cancer |
H351 | Suspected of causing cancer |
H360 | May damage fertility or the unborn child |
H361 | Suspected of damaging fertility or the unborn child |
H361d | Suspected of damaging the unborn child |
H362 | May cause harm to breast-fed children |
H370 | Causes damage to organs |
H371 | May cause damage to organs |
H372 | Causes damage to organs through prolonged or repeated exposure |
H373 | May cause damage to organs through prolonged or repeated exposure |
Environmental hazards | |
Code | Phrase |
H400 | Very toxic to aquatic life |
H401 | Toxic to aquatic life |
H402 | Harmful to aquatic life |
H410 | Very toxic to aquatic life with long-lasting effects |
H411 | Toxic to aquatic life with long-lasting effects |
H412 | Harmful to aquatic life with long-lasting effects |
H413 | May cause long-lasting harmful effects to aquatic life |
H420 | Harms public health and the environment by destroying ozone in the upper atmosphere |
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