Aniline → 1-t-Butoxycarbonyl-3-hydroxy-4-phenylaminopyrrolidine

HRID 2293991

반응식

HRID 2293991 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:12][CH:11]2[O:13][CH:10]2[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[NH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1>C(O)C>[C:1]([O:5][C:6]([N:8]1[CH2:9][CH:10]([NH:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:11]([OH:13])[CH2:12]1)=[O:7])([CH3:2])([CH3:3])[CH3:4]

참가 물질

4

반응물 2

HCID 6115AnilineHCID 10103880tert-Butyl 6-Oxa-3-azabicyclo(3.1.0)hexane-3-carboxylate

생성물 1

HCID 214733471-t-Butoxycarbonyl-3-hydroxy-4-phenylaminopyrrolidine수율 64.5%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

In 20 ml of ethyl alcohol was dissolved 5 g (0.027 mole) of 1-t-butoxycarbonyl-3-epoxypyrrolidine, and 12.6 g (0.135 mole) of aniline was added thereto. The mixture was refluxed by heating for 20 hours. After the mixture was cooled to room temperature, the solvent was removed under reduced pressure, and the residue was applied to silica gel column chromatography (the eluent used was a mixture of ethyl acetate:toluene=1:4) to obtain 4.85 g of 1-t-butoxycarbonyl-3-hydroxy-4-phenylaminopyrrolidine as yellowish brown crystals.

후처리

  1. additionwas added
  2. temperatureThe mixture was refluxed
  3. temperatureby heating for 20 hours
  4. customthe solvent was removed under reduced pressure
  5. additiona mixture of ethyl acetate

출처 및 근거

ORD 기록
ord-cc48a11a0c6f4f92a7fee401fa3e0cd9
출처 데이터셋
uspto-grants-1997_11
특허 번호
US05688791

연결된 노트

불러오는 중…