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Hydrazine hydrate (1:1) → N-benzyloxycarbonyl-3-(1-naphthyl)-L-alanyl-3-(2-thienyl)-DL-alanine hydrazide

HRID 255624
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반응식

HRID 255624 반응식
CO[C:3](=[O:37])[CH:4]([CH2:31][C:32]1[S:33][CH:34]=[CH:35][CH:36]=1)[NH:5][C:6](=[O:30])[C@H:7]([CH2:19][C:20]1[C:29]2[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=2)[CH:23]=[CH:22][CH:21]=1)[NH:8][C:9]([O:11][CH2:12]C1C=CC=CC=1)=[O:10].O.[NH2:39][NH2:40]>CN(C)C=O>[CH2:12]([O:11][C:9]([NH:8][C@H:7]([C:6]([NH:5][CH:4]([C:3]([NH:39][NH2:40])=[O:37])[CH2:31][C:32]1[S:33][CH:34]=[CH:35][CH:36]=1)=[O:30])[CH2:19][C:20]1[C:29]2[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=2)[CH:23]=[CH:22][CH:21]=1)=[O:10])[C:20]1[CH:29]=[CH:24][CH:23]=[CH:22][CH:21]=1
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 13961462N-benzyloxycarbonyl-3-(1-naphthyl)-L-alanyl-3-(2-thienyl)-DL-alanine methyl ester

생성물 1

HCID 13961464N-benzyloxycarbonyl-3-(1-naphthyl)-L-alanyl-3-(2-thienyl)-DL-alanine hydrazide수율 967.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixed solution of 1.0 g (194 mmole) of N-benzyloxycarbonyl-3-(1-naphthyl)-L-alanyl-3-(2-thienyl)-DL-alanine methyl ester and 0.64 g (0.2 mmole) of 80% hydrazine hydrate in 10 ml of dimethylformamide was stirred for 2 hours at room temperature and then left standing overnight at room temperature. Dimethylformamide was removed by evaporation under reduced pressure. Water was added to the residue, and the mixture was stirred to form a powdery precipitate, which was collected by filtration, washed with a mixture of diethyl ether and hexane and dried to yield 1.0 g (100%) of N-benzyloxycarbonyl-3-(1-naphthyl)-L-alanyl-3-(2-thienyl)-DL-alanine hydrazide melting at 163°-164° C.

후처리

  1. waitleft
  2. customDimethylformamide was removed by evaporation under reduced pressure
  3. additionWater was added to the residue
  4. customto form a powdery precipitate, which
  5. filtrationwas collected by filtration
  6. washwashed with a mixture of diethyl ether and hexane
  7. customdried

출처 및 근거

ORD 기록
ord-ca4b8e9e72b84ba2b55b510a852d662a
출처 데이터셋
uspto-grants-1987_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04698329

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