Trifluoroacetic acid → 2-(4-Methoxy-benzyl)-8-((3R,4S)-4-phenyl-pyrrolidin-3-ylmethyl)-2,8-diaza-spiro[4.5]decan-1-one

HRID 1182169노트

반응식

HRID 1182169 반응식
C(OC([N:8]1[CH2:12][C@H:11]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[C@@H:10]([CH2:19][N:20]2[CH2:39][CH2:38][C:23]3([C:27](=[O:28])[N:26]([CH2:29][C:30]4[CH:35]=[CH:34][C:33]([O:36][CH3:37])=[CH:32][CH:31]=4)[CH2:25][CH2:24]3)[CH2:22][CH2:21]2)[CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O.[OH-].[Na+]>ClCCl>[CH3:37][O:36][C:33]1[CH:32]=[CH:31][C:30]([CH2:29][N:26]2[CH2:25][CH2:24][C:23]3([CH2:38][CH2:39][N:20]([CH2:19][C@@H:10]4[C@@H:11]([C:13]5[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=5)[CH2:12][NH:8][CH2:9]4)[CH2:21][CH2:22]3)[C:27]2=[O:28])=[CH:35][CH:34]=1

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 14798Sodium HydroxideHCID 11284019(3S,4S)-3-[2-(4-Methoxy-benzyl)-1-oxo-2,8-diaza-spiro[4.5]dec-8-ylmethyl]-4-phenyl-pyrrolidine-1-carboxylic Acid Tert-Butyl Ester

생성물 1

HCID 114646642-(4-Methoxy-benzyl)-8-((3R,4S)-4-phenyl-pyrrolidin-3-ylmethyl)-2,8-diaza-spiro[4.5]decan-1-one수율 94%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To 5.81 g (10.9 mmol) of (3S,4S)-3-[2-(4-methoxy-benzyl)-1-oxo-2,8-diaza-spiro[4.5]dec-8-ylmethyl]-4-phenyl-pyrrolidine-1-carboxylic acid tert-butyl ester in dichloromethane (100 mL) was added trifluoroacetic acid (30 mL) and the solution was stirred for 1 h at room temperature. The reaction mixture was neutralized with 1N NaOH (40 mL) and extracted with dichloromethane. The organic layer was dried over sodium sulfate and concentrated to give Compound 111 as a white foam (4.42 g, 94%).

후처리

  1. extractionextracted with dichloromethane
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-af80b01275f04a63a494a4964aa43d29
출처 데이터셋
uspto-grants-2007_10
특허 번호
US07288548B2

반응 노트

불러오는 중…