2-Methyl-1-(4-(trifluoromethyl)phenyl)propan-2-amine → Tert-butyl 2-(2-methyl-1-(4-(trifluoromethyl)phenyl)propan-2-yl)hydrazinecarboxylate

HRID 1504294노트

반응식

HRID 1504294 반응식
[CH3:1][C:2]([NH2:15])([CH3:14])[CH2:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]([F:13])([F:12])[F:11])=[CH:6][CH:5]=1.ClC(Cl)(Cl)C1O[N:19]1[C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22]>C(Cl)Cl>[CH3:14][C:2]([NH:15][NH:19][C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])([CH3:1])[CH2:3][C:4]1[CH:5]=[CH:6][C:7]([C:10]([F:11])([F:12])[F:13])=[CH:8][CH:9]=1

참가 물질

4

반응물 2

HCID 1209942-Methyl-1-(4-(trifluoromethyl)phenyl)propan-2-amineHCID 11139943Tert-butyl 3-(trichloromethyl)oxaziridine-2-carboxylate

생성물 1

HCID 89808109Tert-butyl 2-(2-methyl-1-(4-(trifluoromethyl)phenyl)propan-2-yl)hydrazinecarboxylate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

4.2 g of 2-methyl-1-(4-(trifluoromethyl)phenyl)propan-2-amine was dissolved in 30 mL of methylene chloride and mixed with 5.6 g (21 mmol) of separately prepared t-butyl 3-(trichloromethyl)-1,2-oxaziridine-2-carboxylate under cooling with ice. The reaction solution was stirred at room temperature for 30 minutes, washed with 10% aqueous citric acid, with saturated aqueous sodium hydrogen carbonate and with saturated aqueous sodium chloride successively and dried over anhydrous sodium sulfate, and methylene chloride was removed under reduced pressure. The resulting residue was purified by intermediate pressure silica gel column chromatography (silica gel 100 g, ethyl acetate:hexane) to give 1.38 g of the desired product as a white solid.

후처리

  1. temperatureunder cooling with ice
  2. washwashed with 10% aqueous citric acid, with saturated aqueous sodium hydrogen carbonate and with saturated aqueous sodium chloride successively
  3. dry with materialdried over anhydrous sodium sulfate, and methylene chloride
  4. customwas removed under reduced pressure
  5. customThe resulting residue was purified by intermediate pressure silica gel column chromatography (silica gel 100 g, ethyl acetate:hexane)

출처 및 근거

ORD 기록
ord-8d4a54362d5c44198c2cc71536a3f897
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09212348B2

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