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Type
HazMat fee for 500 gram (Estimated)
Excepted Quantity
USD 0.00
Limited Quantity
USD 15-60
Inaccessible (Haz class 6.1), Domestic
USD 80+
Inaccessible (Haz class 6.1), International
USD 150+
Accessible (Haz class 3, 4, 5 or 8), Domestic
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Structure of 2217-65-4 * Storage: {[proInfo.prStorage]}
* 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 tributylphosphine; palladium diacetate In 5,5-dimethyl-1,3-cyclohexadiene for 24 h; Reflux; Inert atmosphere
General procedure: A mixture of fluorobenzene (1.0 mmol), PBu3 (2.0 mmol), Pd(OAc)2 (2 molpercent), K2CO3/ZrO2 (1.5 equiv., based on K2CO3, 2.070 g) in xylene (10 mL) was stirred at reflux under nitrogen for 24 h or according to the TLC. On completion, the resulting mixture was filtered and washed with DCM. The combined organic solvent layers were separated, the solvent evaporated and the product purified by column chromatography with dichloromethane/n-hexane (1:1–1:2) as the eluent to provide the corresponding product 2.
Reference:
[1] Journal of the Chemical Society, Perkin Transactions 2: Physical Organic Chemistry (1972-1999), 1992, # 3, p. 377 - 382
[2] Chemistry - An Asian Journal, 2015, vol. 10, # 2, p. 468 - 473
[3] Journal of Chemical Research, 2016, vol. 40, # 11, p. 691 - 693
[4] Journal of Organic Chemistry, 2018, vol. 83, # 24, p. 14882 - 14893
2
[ 1493-27-2 ]
[ 88-75-5 ]
[ 2217-65-4 ]
Reference:
[1] Synthesis, 1996, # 8, p. 930 - 940
[2] Zeitschrift fur Anorganische und Allgemeine Chemie, 2015, vol. 641, # 1, p. 128 - 135
3
[ 88-73-3 ]
[ 2217-65-4 ]
Reference:
[1] Chemistry - An Asian Journal, 2015, vol. 10, # 2, p. 468 - 473
4
[ 298-14-6 ]
[ 1493-27-2 ]
[ 2217-65-4 ]
Reference:
[1] Journal of Organic Chemistry, 1984, vol. 49, p. 1122 - 1125
[2] Journal of Organic Chemistry, 1984, vol. 49, p. 1122 - 1125
5
[ 101-84-8 ]
[ 2217-65-4 ]
[ 101-63-3 ]
[ 5950-83-4 ]
Reference:
[1] Journal of Organic Chemistry, 1981, vol. 46, # 15, p. 3056 - 3060
6
[ 100-02-7 ]
[ 126813-47-6 ]
[ 2217-65-4 ]
Reference:
[1] Patent: US4880821, 1989, A,
7
[ 95-56-7 ]
[ 1493-27-2 ]
[ 2217-65-4 ]
Reference:
[1] Australian Journal of Chemistry, 1988, vol. 41, # 6, p. 995 - 1001
Reference:
[1] Journal of the Chemical Society, 1934, p. 716,719
19
[ 119-66-4 ]
[ 2217-65-4 ]
Reference:
[1] Comptes Rendus Hebdomadaires des Seances de l'Academie des Sciences, 1928, vol. 186, p. 955[2] Bulletin de la Societe Chimique de France, 1928, vol. <4> 43, p. 838
20
[ 55144-24-6 ]
[ 88-73-3 ]
[ 2217-65-4 ]
Reference:
[1] Chemische Berichte, 1896, vol. 29, p. 2084[2] Chemische Berichte, 1897, vol. 30, p. 738 Anm. 2
21
[ 151-50-8 ]
[ 528-29-0 ]
[ 2217-65-4 ]
Reference:
[1] Recueil des Travaux Chimiques des Pays-Bas, 1904, vol. 23, p. 32
22
[ 2217-65-4 ]
[ 24878-25-9 ]
Yield
Reaction Conditions
Operation in experiment
85%
With hydrogenchloride; iron In water for 24 h; Reflux
General procedure: A suspension of iron powder and HCl in water was stirred and refluxed for 25 min. Then, the corresponding dinitro compound was added to this hot suspension and the mixture was refluxed for 24 h. The mixture was allowed to reach room temperature and hydrolyzed with 20 mL of NaOH 2.5 M and, extracted with chloroform (2 20 mL). The organic phase was dried with Na2SO4 and evaporated to yield the diamino compounds as solids.
Reference:
[1] Tetrahedron, 1995, vol. 51, # 2, p. 579 - 590
[2] Polyhedron, 2015, vol. 90, p. 165 - 174
[3] Synthesis, 1996, # 8, p. 930 - 940
[4] Journal of Organic Chemistry, 1994, vol. 59, # 24, p. 7306 - 7315
[5] Zeitschrift fur Anorganische und Allgemeine Chemie, 2015, vol. 641, # 1, p. 128 - 135
[6] Yakugaku Zasshi, 1955, vol. 75, p. 1077,1079[7] Chem.Abstr., 1956, p. 5618
[8] Chemische Berichte, 1897, vol. 30, p. 738
[9] Journal of Organic Chemistry, 1961, vol. 26, p. 1901 - 1907
[10] Journal of Organic Chemistry, 1962, vol. 27, p. 4098 - 4101
[11] Angewandte Chemie, 1993, vol. 105, # 8, p. 1254 - 1256
[12] Journal of Molecular Structure, 2003, vol. 645, # 1, p. 51 - 59
With hydrogenchloride; iron; In water; for 24h;Reflux;
General procedure: A suspension of iron powder and HCl in water was stirred and refluxed for 25 min. Then, the corresponding dinitro compound was added to this hot suspension and the mixture was refluxed for 24 h. The mixture was allowed to reach room temperature and hydrolyzed with 20 mL of NaOH 2.5 M and, extracted with chloroform (2 20 mL). The organic phase was dried with Na2SO4 and evaporated to yield the diamino compounds as solids.
With tributylphosphine; palladium diacetate; In 5,5-dimethyl-1,3-cyclohexadiene; for 24h;Reflux; Inert atmosphere;
General procedure: A mixture of fluorobenzene (1.0 mmol), PBu3 (2.0 mmol), Pd(OAc)2 (2 mol%), K2CO3/ZrO2 (1.5 equiv., based on K2CO3, 2.070 g) in xylene (10 mL) was stirred at reflux under nitrogen for 24 h or according to the TLC. On completion, the resulting mixture was filtered and washed with DCM. The combined organic solvent layers were separated, the solvent evaporated and the product purified by column chromatography with dichloromethane/n-hexane (1:1-1:2) as the eluent to provide the corresponding product 2.
{2-[2-(2-Methoxy-acetylamino)-phenoxy]-phenylamino}-acetic acid 2-({2-[2-(2-methoxy-acetylamino)-phenoxy]-phenylcarbamoyl}-methoxy)-ethyl ester[ No CAS ]
EXAMPLE 5 Reaction of potassium ortho-nitrophenate having the formula: STR18 with ortho-nitrofluorbenzene, in order to prepare 2,2'-dinitrodiphenyl ether having the formula: STR19 in the presence of tris-(3,6,9-trioxadecyl)-amine in o-dichlorobenzene.
α-(bromomethyl)-4-(1H-imidazol-1-yl)benzenemethanol[ No CAS ]
[ 2217-65-4 ]
[ 14321-27-8 ]
α-[[Ethyl(phenylmethyl)amino]methyl]-4-(1H-imidazol-1-yl)-benzenemethanol phosphoric acid salt[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
With phosphoric acid; In tetrahydrofuran; methanol; ethanol; dichloromethane;
Example 44 α-[[Ethyl(phenylmethyl)amino]methyl]-4-(1H-imidazol-1-yl)-benzenemethanol phosphoric acid salt Add α-(bromomethyl)-4-(1H-imidazol-1-yl)benzenemethanol (7.80 g, 29.2 mmol) to a room temperature solution of N-ethylbenzylamine (21.7 mL, 146.0 mmol) in tetrahydrofuran (75 mL). Reflux the resultant mixture for about 5.5 days. Cool to room temperature and concentrate in vacuo. Chromatograph the resultnat residue on alumina (neutral, activity III, 500 g) using first methylene chloride then 2.5% methanol in methylene chloride as eluent. Collect the product fractions and concentrate in vacuo. The residue is dissolved in ethanol and phosphoric acid added until the pH is 2.5. Concentration in vacuo affords the title compound. NMR (D2 O/TSP): δ=1.43(t,3), 3.44(m,4), 4.49(m,2), 5.10(br s,1), 7.41-7.85(m,11), and 9.06(s,1; exchangeable with D2 O) ppm. EtOH at 1.16 and 3.65 ppm.
Step 1: N-(2-Dimethylaminoethyl)-N-methyl-4-(4-nitrophenoxy)-3-nitrobenzenesulfonamide To a solution of N-(2- dimethylaminoethyl)-N-methyl-4- chloro-3-nitrobenzenesulfonamide (2.2 g, 6.84 mmol) and 4- nitrophenol (0.97 g, 7.0 mmol) in dimethylformamide (30 mL) was added 60% sodium hydride-mineral oil suspension (0.28 g, 7.0 mmol). The resulting solution was stirred at 60 for 20 hours under N2. After concentrating under reduced pressure at 50, the residue was partitioned between ethyl acetate and water. The ethyl acetate extract was washed with brine, dried (Na2 SO4), filtered and concentrated. The residue was flash chromatographed over silica gel and 2.8 g of the nitrophenyl ether eluted with 3% methanol-97% chloroform.
To a solution of N-(2tert.butoxycarbonylaminoethyl)-N-methyl-4-chloro-3-nitrobenzenesulfon amide (1.5 g, 3.81 mmol) and 4-nitrophenol (0.53 g, 3.81 mmol) in dimethylformamide (30 mL) was added 60% sodium hydride-mineral oil suspension (0.15 g, 3.81 mmol). The resulting solution was stirred at 20-25 under nitrogen for 3 days. After concentrating under reduced pressure at 55, the residue was partitioned between ethyl acetate and 1 M acetic acid. The ethyl acetate extract was washed with sodium bicarbonate solution, brine and dried (Na2 SO4). After filtering and concentrating under reduced pressure, the residue was flash chromatographed over silica gel. Elution with chloroform gave 2.0 g of the 4 nitrophenyl ether containing some unreacted chloro compound.
With sodium ethanolate; In methanol; at 45 - 80℃; for 1.25h;Large scale;
Add 150 kg of o-nitrochlorobenzene to a 2000L reactor, add 150 kg of methyl alcohol, start stirring to warm up, and when the temperature rises to 48 , start adding the sodium ethoxide solution purchased, according to the concentration of sodium ethoxide purchased (Content 30%) calculate the addition, the addition amount is 1 ~ 1.01 (molar ratio with o-nitrochlorobenzene), the control temperature is not lower than 45 C, not higher than 55 after adding sodium ethoxide solution. Then close all inlets and outlets on the reactor, raise the temperature to 80 C, the pressure in the reactor is 2.5 ~ 3.5 × 104Pa, and keep it warm for 75 minutes. Then start to distill ethanol at this temperature, while maintaining the temperature, continue to slowly add the recovered washing water, washing the generated sodium chloride, and the amount of washing water added is 300 kg. Then cool down to room temperature. After the product and moisture have dried, the material is dried. The obtained product was 157.3 kg; the melting point of the product was 2.0 C., the product purity: 99.7% (chromatographic analysis); p-nitrophenol: 0.02%; the yield was 98.9%.