* 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.
With sodium nitrite In 1,2-dichloro-ethane at 110℃; for 60 h; Sealed tube
It was added in a closed reaction vessel 0.3mmol 2-amino-6-chlorobenzothiazole, 0.6mmol sodium nitrite, 3mL1,2- dichloroethane,the reaction mixture was stirred at 110 reaction conditions 60 hours.After the reaction was stopped, cooled to room temperature, the reactionmixture was added 10mL diluted with dichloromethane, filtration and stripped ofsolvent under reduced pressure, the residue was purified by columnchromatography, eluent V (petroleum ether) / V (ethyl ester) = 6/1, to give6-chlorobenzothiazole, yield 89percent.
59%
Stage #1: With phosphoric acid; sodium nitrite In water at -10℃; for 2 h; Stage #2: With hypophosphorous acid In water at -5 - 20℃;
General procedure: Thiazoles (1b-f, j) were prepared from 2-aminothiazoles according to the reported procedure with slight modifications. 24 To a mechanically-stirred solution of 2-amino-6-chlorobenzothiazole (4 g, 21.7 mmol, 1.0 equiv) in 84percent aq phosphoric acid (80 mL) was added a solution of sodium nitrite (9.0 g, 13 mmol, 6.0 equiv) in water (28 mL) dropwise below the surface at -10 °C. After stirring at -10 °C for another 2 h, a 50percent aq solution of hypophosphorous acid (60 mL) was added dropwise to the resulting thick syrup mixture at -5 °C. The reaction mixture was warmed to room temperature, stirred overnight, and then diluted with water (300 mL). Na2CO3 was added portionwise to adjust to pH=8 and extracted with DCM. The organic phase was dried over Na2SO4, concentrated under vacuum, and purified over column chromatography (petroleum ether/EtOAc=100:1) to give 6-chlorobenzothiazole as white solid (2.2 g, 59percent yield).
Reference：
[1] Chemical and Pharmaceutical Bulletin, 1998, vol. 46, # 4, p. 623 - 630
[2] Patent: CN105367442, 2016, A, . Location in patent: Paragraph 0018
[3] Chemical and Pharmaceutical Bulletin, 1997, vol. 45, # 9, p. 1547 - 1549
[4] Tetrahedron, 2013, vol. 69, # 22, p. 4436 - 4444
[5] Synthetic Communications, 1980, vol. 10, # 3, p. 167 - 174
[6] Journal of Heterocyclic Chemistry, 2000, vol. 37, # 6, p. 1655 - 1658
[7] Chemical Communications, 2012, vol. 48, # 42, p. 5181 - 5183
[8] Organic Letters, 2013, vol. 15, # 17, p. 4600 - 4603
[9] Tetrahedron, 2014, vol. 70, # 2, p. 245 - 250
[10] Organic and Biomolecular Chemistry, 2017, vol. 15, # 7, p. 1606 - 1611
2
[ 23474-98-8 ]
[ 124-38-9 ]
[ 2942-10-1 ]
Yield
Reaction Conditions
Operation in experiment
72%
Stage #1: With 1,8-diazabicyclo[5.4.0]undec-7-ene In 1-methyl-pyrrolidin-2-one at 70℃; for 0.5 h; Schlenk technique Stage #2: With phenylsilane In 1-methyl-pyrrolidin-2-one at 60℃; for 18 h; Schlenk technique
General procedure: A tube-type Schlenk flask was charged with 0.045 mmol of catalyst D, 0.045 mmol of 1,8-diazabicyclo[5.4.0]undec-7-ene (7μL), and 1mL of N-methylpyrrolidone. The solution was stirred under nitrogen atmosphere at 60–70°C for 30 min. And, 2mL of N-methylpyrrolidone was added, followed by addition of a balloon charged with carbon dioxide gas. The solution was stirred at 60–70°C for 30 min. Then, 2-aminobenzenethiol derivatives (0.5 mmol), phenylsilane (1.5 mmol) dissolved in 0.5mL of N-methylpyrrolidone was added to the mixture. Reaction was carried out at 60–70°C for 18–30h. After the solution was cooled to room temperature, purification by flash chromatography on silica gel with n-hexane and ethyl acetate afforded benzothiazole derivatives.
With sodium nitrite; In 1,2-dichloro-ethane; at 110℃; for 60h;Sealed tube;
It was added in a closed reaction vessel 0.3mmol 2-amino-6-chlorobenzothiazole, 0.6mmol sodium nitrite, 3mL1,2- dichloroethane,the reaction mixture was stirred at 110 reaction conditions 60 hours.After the reaction was stopped, cooled to room temperature, the reactionmixture was added 10mL diluted with dichloromethane, filtration and stripped ofsolvent under reduced pressure, the residue was purified by columnchromatography, eluent V (petroleum ether) / V (ethyl ester) = 6/1, to give6-chlorobenzothiazole, yield 89%.
88%
With isopentyl nitrite; In tetrahydrofuran; at 120℃; under 5250.53 Torr; for 0.333333h;
General procedure: A solution of the selected heterocyclic starting material (1.00 mmol) in THF (10 mL) and a solutionof isopentyl nitrite (141 mg, 1.20 mmol) in THF (10 mL) were both pumped at a flow rate of 0.25 mLmin1 with a Vapourtech ?Easy MedChem V3? system, meeting at a PTFE T-piece and the outputflowing through a 10.0 mL coil reactor maintained at 120 C, giving a residence time of 20 min.The pressure of the system was maintained at 7 bar with a back-pressure regulator. For compoundswhere an isolated yield was reported: the output mixture was concentrated under reduced pressureto give an oil (or powder). The oil (or powder) was purified using column chromatography withvarious mixtures of ethyl acetate and hexane as the eluent, or by recrystallisation using methanol, togive isolated compounds that showed no impurities by NMR spectroscopy. For compounds where aconversion was reported (due to volatility of products), the output mixture was carefully concentratedunder a reduced pressure of 100 mbar for 10 min and the conversion was calculated by integration ofproduct peaks to a quantified internal standard (nitrobenzene).
59%
General procedure: Thiazoles (1b-f, j) were prepared from 2-aminothiazoles according to the reported procedure with slight modifications. 24 To a mechanically-stirred solution of 2-amino-6-chlorobenzothiazole (4 g, 21.7 mmol, 1.0 equiv) in 84% aq phosphoric acid (80 mL) was added a solution of sodium nitrite (9.0 g, 13 mmol, 6.0 equiv) in water (28 mL) dropwise below the surface at -10 C. After stirring at -10 C for another 2 h, a 50% aq solution of hypophosphorous acid (60 mL) was added dropwise to the resulting thick syrup mixture at -5 C. The reaction mixture was warmed to room temperature, stirred overnight, and then diluted with water (300 mL). Na2CO3 was added portionwise to adjust to pH=8 and extracted with DCM. The organic phase was dried over Na2SO4, concentrated under vacuum, and purified over column chromatography (petroleum ether/EtOAc=100:1) to give 6-chlorobenzothiazole as white solid (2.2 g, 59% yield).
With isopentyl nitrite; In tetrahydrofuran; for 0.5h;Reflux;
General procedure: A 50 mLSchlenk tube was charged with 2-aminobenzothiazole derivative (6.5 mmol) and 10mL of THF, and then isoamyl nitrite (14.3 mmol) was added slowly into thesolution. The resultant mixture was refluxed for 30 minutes, and poured intoice-water, and the resultant aqueous mixture was extracted with ethyl acetate(3×30 mL). The organic extracts were combined and washed with brine, dried overMgSO4, filtered, concentrated in vacuum andpurified by column chromatography, giving the desired benzothiazoles in similaryields with the reported procedure.
With water; caesium carbonate; for 0.166667h;Microwave irradiation;
General procedure: Add 2 ml of water to the microwave reactor,1 mmol of benzothioamide and 0.2 mmol of cesium carbonate,Reacted at a fixed power of 120 W for 10 min,Extracted with ethyl acetate and concentrated under reduced pressure.To give a pale yellow solid, yield 99%.
With hydridotetakis(triphenylphosphine)rhodium(I); 1,2-bis-(diphenylphosphino)ethane; In chlorobenzene; for 3h;Inert atmosphere; Reflux;
General procedure: In a two-necked flask equipped with a reflux condenser were placed RhH(PPh3)4 (4 mol%, 11.5 mg), 1,2-bis(diphenylphosphino)ethane (8 mol%, 8.0 mg), 1,3-benzothiazole 5 (0.25 mmol, 27.3 mL), and (alpha-phenylthio)isobutyrophenone 6 (0.25 mmol, 64.0 mg) in chlorobenzene (0.25 mL) under an argon atmosphere, and the solution was heated at reflux for 3 h. The mixture was purified by flash column chromatography on silica gel giving 7 (55.8 mg, 92%) and isobutyrophenone 8 (34.3 mg, 93%) with the recovery of 5 (3.5 mg, 10%) and 6 (0.8 mg, 1%).
With palladium diacetate; copper(II) dipivaloate; caesium carbonate; copper(I) bromide; In 1,4-dioxane; dimethyl sulfoxide; at 110℃; for 12h;Schlenk technique; Inert atmosphere;
General procedure: A flame-dried 25-mL Schlenk flask equipped with a magnetic stir bar was charged with Pd(OAc)2 (11.2 mg, 0.05 mmol, 10 mol %), copper(II) pivalate (400 mg, 1.5 mmol, 3.0 equiv), Cs2CO3 (163 mg, 0.5 mmol, 1.0 equiv), pyridine N-oxide (190 mg, 2.0 mmol, 4.0 equiv), and CuBr (7 mg, 0.05 mmol, 10 mol %). The flask was fitted with a rubber septum, evacuated, and refilled with argon (repeating three times). Dioxane/DMSO (19:1, 4.0 mL) and benzothiazole (67.3 mg, 0.5 mmol, 1.0 equiv) were added via syringes under an atmosphere of N2. The septum was then replaced by a Teflon-coated screw cap under N2. The reaction mixture was stirred at room temperature for 15 min and then in a preheated oil bath (at 110 C) for 12 h, cooled down to room temperature, diluted with DCM (15 mL) and filtered through a Celite pad. The filtrate was then washed twice with 10-20 mL of DCM. The combined organic extracts were washed with 5 mL of saturated NH4Cl aq solution (containing 1% v/v ammonium hydroxide) to remove the residual copper(II). The blue aqueous phase was extracted with DCM (15 mL×3). The combined organic phase was dried over Na2SO4, concentrated under vacuum, and purified by column chromatography on silica gel (eluent: DCM/acetone=20:1) to provide the desired product 3a as a pale yellow solid (75 mg, 67% yield).
(6-chlorobenzo[d]thiazol-2-yl)(phenyl)methanone[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
75%
With iron(III) chloride hexahydrate; oxygen; tricyclohexylphosphine tetrafluoroborate; In water; dimethyl sulfoxide; at 120℃; for 20h;
General procedure: A 10 mL reaction tube was charged with FeCl3·6H2O (2.7 mg, 0.01 mmol), P(Cy)3·HBF4 (3.7 mg, 0.01 mmol), benzothiazole (1a, 21.8 muL, 0.2 mmol), acetophenone (2a, 35 muL, 0.3 mmol), HO 2(0.1 mL) and DMSO (0.3 mL). The reaction vessel was flushed with oxygen for three times and sealed. The resulting solution was heated to 120 oC for 20 h. After cooling to room temperature, the volatiles were removed under vacuum and the residue was purified by column chromatography (silica gel, petroleum ether/ethyl acetate = 98:2) to give 3a as a yellow solid; yield: 35.9 mg (75%).
With [1,3-bis(2,6-diisopropylphenyl)imidazol-2-ylidene]copper(I) iodide; potassium carbonate; In N,N-dimethyl-formamide; at 140℃; for 3h;
General procedure: The following provide the typical experimental procedure for the direct C-H thiolation ofbenzothiazole with thiophenol. To the 5 mL of test tube containing a magnetic stirrer bar was placed(IPr)CuI (29 mg, 0.05 mmol) and K2CO3 (69mg, 0.50 mmol)and subsequently added benzothiazole(mg, 0.25 mmol)thiophenol (mg, 0.50 mmol) in DMF (1.5 mL). The resulting mixture was heated at140 C for 3h. After the mixture was allowed to cool to room temperature, water (1 mL) was addedand the solution was extracted with three portions of 10 mL ethyl acetate. GC/MS analysis revealedthe presence of 2-phenylthiobenzothiazole. The organic layer was dried (MgSO4), filtered, and thesolvent was removed by rotary evaporator in vacuo. The residue was subjected to preparative TLC(hexane/ethyl acetate = 5/1) to give the pure product
With dipotassium peroxodisulfate; iron(III) chloride hexahydrate; In water; dimethyl sulfoxide; at 100℃; for 12h;
General procedure: A dried reflux tube equipped witha magnetic stir bar charged with benzothiazole derivative (0.5 mmol 1.0equiv), benzylalcohol derivative (1.5mmol 3.0equiv), FeCl3·6H2O (0.1equiv), K2S2O8 (2.0 equiv), DMSO/H2O (2:1 mL) and the reaction vessel was placedin a 100C oil bath for 12 h under air. After cooling to room temperature,the mixture was diluted with ethyl acetate and directly filtered through a padof celite and washed with water. The organic phase was dried over NaSO4and removed under reduced vacuum. The residue was purified by columnchromatography eluting with ethyl acetate and hexane to afford thedesired product.
(6-chlorobenzo[d]thiazol-2-yl)(phenyl)methanone[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
With dipotassium peroxodisulfate; iron(III) chloride hexahydrate; In water; dimethyl sulfoxide; at 100℃; for 12h;
General procedure: A dried reflux tube equipped witha magnetic stir bar charged with benzothiazole derivative (1 mmol 2.0 equiv), acetophenone derivative (0.5 mmol 1.0equiv),FeCl3·6H2O (0.2equiv), K2S2O8 (3.0 equiv), DMSO/H2O (2:1 mL)and the reaction vessel was placed in a 100C oil bath for 12 h under air.After cooling to room temperature, the mixture was diluted with ethyl acetateand directly filtered through a pad of celite and washed with water. Theorganic phase was dried over NaSO4 and removed under reduced vacuum.The residue was purified by column chromatography eluting with ethyl acetateand hexane to afford the desired product
General procedure: A tube-type Schlenk flask was charged with 0.045 mmol of catalyst D, 0.045 mmol of 1,8-diazabicyclo[5.4.0]undec-7-ene (7muL), and 1mL of N-methylpyrrolidone. The solution was stirred under nitrogen atmosphere at 60-70C for 30 min. And, 2mL of N-methylpyrrolidone was added, followed by addition of a balloon charged with carbon dioxide gas. The solution was stirred at 60-70C for 30 min. Then, 2-aminobenzenethiol derivatives (0.5 mmol), phenylsilane (1.5 mmol) dissolved in 0.5mL of N-methylpyrrolidone was added to the mixture. Reaction was carried out at 60-70C for 18-30h. After the solution was cooled to room temperature, purification by flash chromatography on silica gel with n-hexane and ethyl acetate afforded benzothiazole derivatives.
1-methyl-2-oxo-1,2-dihydroquinolin-4-yl trifluoromethanesulfonate[ No CAS ]
C17H11ClN2OS[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
49%
With copper(l) iodide; palladium(II) trifluoroacetate; potassium carbonate; tricyclohexylphosphine; In 5,5-dimethyl-1,3-cyclohexadiene; at 140℃; for 12h;Inert atmosphere;
General procedure: 1 mL Xylene was added into the flask charged with 0.25 mmol 4-quinolinonyl triflate, 0.75 mmol benzothiazole, 5 mol% Pd(TFA)2 (4.1 mg), 20 mol% PCy (14 mg), 0.25 mmol K2CO3, 10 mol% CuI (4.7 mg). The mixture was stirred at 140oC under Ar for 12 hours, then cooled down to room temperature, diluted with 20 mL ethyl acetate and washed with 10 mL H2O. The aqueous layer was extracted twice with ethyl acetate (5 mL) and the combined organic phase was dried over Na2SO4. After evaporation of the solvents the residue was purified by flash column chromatography (silica gel, PE/EtOAc) to afford the desired products 3 and 5.
With 1,3-bis-(diphenylphosphino)propane; caesium carbonate; palladium dichloride; In acetonitrile; at 85℃; for 36h;Green chemistry;
A 2-arylbenzothiazole compound preparation method, the method is to successively add <strong>[2942-10-1]6-chlorobenzothiazole</strong>, 2-fluorophenyl(phenyl)iodonium tetrafluoroborate, palladium chloride, 1,3-bis(diphenylphosphino)propane and caesium carbonate into reaction solvent acetonitrile. At 85C, react for 36 hours.Wherein: bromination arrowhead with 6 - chlorobenzene and thiazole molar ratio of 1:100, 6 - chlorobenzene and thiazole with 2 - fluorophenyl (phenyl) four boron fluoride Iodized salt molar ratio of 1: 2.5, 6 - chlorobenzene and thiazole with 1, 3 - double-(diphenylphosphine) propane molar ratio of 1:100, 6 - chlorobenzene and thiazole with cesium carbonate in a molar ratio of 1: 2.5, 6 - chlorobenzene and thiazole with acetonitrile in a molar ratio of 1:360.The whole reaction process according to the embodiment 1 of the thin-layer chromatography tracking obtained reaction liquid; the reaction solution according to the embodiment 1 the method sequentially through the extraction, drying, concentration, after the column chromatography, to obtain 6-chloro-2-(2-fluorophenyl)benzothiazole, yield is 75%.
With copper(l) chloride; In chlorobenzene; at 130℃; for 12h;Schlenk technique; Inert atmosphere;
In a pressure-resistant Schlenk tube, cuprous chloride (0.05 mmol) was charged,6-chlorobenzothiazepine (0.5 mmol),The system was evacuated and replaced with argon three times,Under gas protection,The di-tert-butyl peroxide (2 mmol) was added successively to a micro-And chlorobenzene (2 ml),The system was then sealed and heated at 130 C in an oil bath for 12 hours,After completion of the reaction, the solvent was distilled off under reduced pressure,Concentrated by a simple column chromatography (eluent using petroleum ether (60 to 90 C) mixed with ethyl acetate)To give the product 6-chloro-N-methylbenzothiazolin-2-one (81 mg)The yield was 81%.
In the reaction flask, Under argon, a catalyst (9.9 mg, 0.025 mmol, 5 mol%), potassium tert-butoxide (0.0672 g, 0.6 mmol) DMF (3.0 ml), <strong>[2942-10-1]6-chlorobenzothiazole</strong> (84.99 mg, 0.5 mmol) was added to the carbon dioxide gas, and the reaction was stirred at 80 C for 18 hours under normal pressure. Cooled to 65 C, methyl iodide (93 mul, 1.5 mmol) was added, The reaction was stirred at 65 C for 1 hour. Cooled to room temperature, the reaction was terminated with deionized water, The reaction product was extracted with ethyl acetate and purified by column chromatography (Using a mixed solvent of ethyl acetate / petroleum ether in a volume ratio of 1:10 as a developing solvent) The yield was 75%.
General procedure: Under an air atmosphere, a sealable reaction tube with a Teflon-coated screw cap equipped with a magnetic stir bar was charged with benzothiazole 1 (1.0 mmol), toluene derivative 2 (3.0 mmol), and Cu(OTf)2 (0.10 mmol) in DCE/DMSO (5:1, 2.0 mL). To this was added 70% aq TBHP (6.0 equiv) at r.t. The rubber septum was then replaced by a Teflon-coated screw cap, and the reaction vessel placed in an oil bath at 90 C for 24 or 36 h. When the reaction was complete, it was cooled to r.t. and monitored by TLC. To the resulting solution was added 98% hydrazine hydrate (0.5 or 1.0 mL), K2CO3 (3.0 mmol), and EtOH(2.0 mL), the mixture was stirred for 5 min and then poured into 10% HCl (15 mL); the mixture was extracted with EtOAc (2 ×). The combined organic layers were dried (anhyd Na2SO4) and the solvents were removed in vacuo. The residue was purified by flash chromatography (silica gel, petroleum ether/EtOAc 20:1) to give the product.
2-(4-(p-tolyl)-1H-1,2,3-triazol-1-yl)benzoic acid[ No CAS ]
6-chloro-2-(2-(4-(p-tolyl)-1H-1,2,3-triazol-1-yl)phenyl)benzo[d]thiazole[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
60%
With triphenylphosphine; silver carbonate; palladium dichloride; In dimethyl sulfoxide; at 150℃; for 12h;Inert atmosphere; Sealed tube;
General procedure: 2-(4-(p-Tolyl)-1H-1,2,3-triazol-1-yl)benzoic acid 1a (0.45 mmol), benzo[d]thiazole 2a (0.3 mmol), PdCl2 (5.3 mg, 0.03 mmol), Ag2CO3 (248.2 mg, 3.0 equiv), PPh3 (15.7 mg, 0.06 mmol) and DMSO (1 mL) were sequentially added to a 15mL pressure tube. Then the tube was sealed and stirred at 150 C for 12 h. After consumption of the 1,4-disubstitued 1,2,3-triazoles monitored by TLC analysis, H2O (15 mL) was added to the mixture and extracted with EtOAc in 3 times (3x15mL). The combined organic layers were washed with brine (3x5mL), dried with Na2SO4, and concentrated under reduced pressure to afford the crude product. Purification by column chromatography on silica gel with EtOAc-PE (1:8) afforded the desired product 3a.
With 1.3-propanedithiol; dimethyl sulfoxide; potassium hydroxide; at 130℃; for 12h;Inert atmosphere;
General procedure: To a solution of benzothiazoles or benzoxazoles (1, 1 mmol) in DMSO (3 mL), was added KOH (280 mg, 5 equiv) and 1,3-propanedithiol (207 muL, 2 mmol). The reaction mixture was heated under argon at 130 C for 12 h. After cooling to room temperature, water (10 mL) was added. The pH of the reaction mixture was adjusted to 3-4 using 5% HCl. The resulting mixture was extracted with ethyl acetate (15 mL ×2). The organic layer was washed with water and brine, dried over anhydrous MgSO4 and concentrated using rotary evaporator. The crude product was purified by silica gel column chromatography using ethyl acetate/n-hexane as eluent to afford the corresponding heteroaryl thiols 3.
With dipotassium hydrogenphosphate; dichloro(dimethylglyoxime)(dimethylglyoximato)cobalt(III); 9-(2-mesityl)-10-methylacridinium perchlorate; In water; 1,2-dichloro-ethane; at 25 - 30℃; for 24h;Inert atmosphere; Irradiation; Schlenk technique;
General procedure: To an oven-dried 10 mL vial were added the heteroarene 1 (0.40 mmol, 1.0 equiv), 1-adamantanecarboxylic acid (2; 216 mg, 1.20 mmol, 3.0 equiv), K2HPO4 (209 mg, 1.20 mmol, 3.0 equiv), 9-mesityl-10-methylacridinium perchlorate (8.2 mg, 5.0 mol%), and [Co(dmgH)(dmgH2)Cl2] (11.6 mg, 8.0 mol%). After the vial was capped with a septum, it was evacuated and refilled with N2 for three times before DCE (1.5 mL) and H2O (0.5 mL) were added sequentially. If the heterocyclic substrate 1 was a liquid, it was added at this point. The mixture was degassed and stirred for 24 h under visible light irradiation (Kessil A360N, see Figure S-1 in the Supporting Information). After 24 h, the mixture was diluted with CH2Cl2 (10 mL) and H2O (10 mL), and the phases were separated. The aqueous layer was extracted with CH2Cl2 (2 × 10 mL), the combined organic phases were dried (Na2SO4), and the solvent was removed under reduced pressure. The residue was purified by column chromatography on silica gel (n-pentane or n-hexane/Et2O 20:1 to 2:1) affording the corresponding product 3.
With hydrogenchloride; tetra-n-butyl-ammonium chloride In lithium hydroxide monohydrate at 30℃; for 24h; Irradiation;
5 Example 5 2-(2-(6-Chlorobenzothiazol-2-yl)-5-oxopyrrolidin-1-yl)acetamide (IV-e)
Compound (I) 6-chlorobenzothiazole (33.8 mg, 0.2 mmol), compound (III) pyracetamide (284 mg, 2 mmol), tetrabutylammonium chloride (22.2 mg) were added to a reaction tube equipped with magnetic stirring , 0.08mmol) and a mass fraction of 37% concentrated hydrochloric acid (39.5mg, 0.4mmol), water (2.0mL) was added to the mixture, the reaction system was irradiated under violet light with a power of 25W, and the reaction was stirred at 30°C for 24 hours, The reaction solution was quenched with saturated sodium bicarbonate, washed with saturated brine, and the mixture was extracted with ethyl acetate. The combined organic layers were dried over anhydrous Na 2 SO 4 and concentrated under reduced pressure. The crude product was purified on a silica gel column using a volume ratio of 30:1 dichloromethane/methanol to obtain the desired product in 38% yield and 98.3% HPLC purity.
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