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HCID 86713334, 화합물 → HCID 66569359, 화합물

HRID 928005
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인쇄 미리보기

반응식

HRID 928005 반응식
[CH2:1]([O:8][C:9]([N:11]([C@H:13]1[CH2:17][CH2:16][N:15](C(OC(C)(C)C)=O)[CH2:14]1)[CH3:12])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>FC(F)(F)C(O)=O.C(Cl)Cl>[CH3:12][N:11]([C@H:13]1[CH2:17][CH2:16][NH:15][CH2:14]1)[C:9](=[O:10])[O:8][CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 86713334HCID 86713334, 화합물2회

생성물 1

HCID 66569359HCID 66569359, 화합물수율 115.1%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 6422Trifluoroacetic acid용매

실험 절차

A solution of tert-butyl (S)-3-(N-benzyloxycarbonyl-N-methylamino)pyrrolidine-1-carboxylate (Intermediate 130, 1.81 g) in trifluoroacetic acid (8 mL) and DCM (8 mL) was left to stand at room temperature for 30 minutes. The resultant mixture was concentrated in vacuo and the residue was dissolved in DCM and brine, basified with 2M sodium hydroxide and filtered through a phase separator. The filtrate was concentrated in vacuo to give benzyl N-methyl-(S)-pyrrolidin-3-ylcarbamate (1.46 g) as a light coloured oil.

후처리

  1. concentrationThe resultant mixture was concentrated in vacuo
  2. dissolutionthe residue was dissolved in DCM
  3. filtrationfiltered through a phase separator
  4. concentrationThe filtrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-cf5895ddea674dee90de3581593ade40
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09290472B2

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