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P,P-Diphenylphosphinic azide → HCID 178445900, 화합물

HRID 1607417
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HRID 1607417 반응식
[C:1]1([CH2:11][CH:12]([CH2:16][CH:17]=[CH:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[C:13](O)=[O:14])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.[NH2:25][C@H:26]([C:33]([NH:35][C@H:36]([CH:41]=[N:42][NH:43][C:44]([NH2:46])=[O:45])[CH2:37][CH:38]([CH3:40])[CH3:39])=[O:34])[CH2:27][C:28]1[N:32]=[CH:31][NH:30][CH:29]=1.C1(P(N=[N+]=[N-])(C2C=CC=CC=2)=O)C=CC=CC=1.C(=O)(O)[O-].[Na+]>CN(C)C=O.C(N(CC)CC)C>[C:1]1([CH2:11][CH:12]([CH2:16][CH:17]=[CH:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[C:13]([NH:25][C@H:26]([C:33]([NH:35][C@H:36]([CH:41]=[N:42][NH:43][C:44]([NH2:46])=[O:45])[CH2:37][CH:38]([CH3:40])[CH3:39])=[O:34])[CH2:27][C:28]2[N:32]=[CH:31][NH:30][CH:29]=2)=[O:14])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

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HCID 199401P,P-Diphenylphosphinic azideHCID 516892Sodium BicarbonateHCID 53925726(+/-)-2-(1-Naphthylmethyl)-5-phenyl-4-pentenoic acidHCID 178445905HCID 178445905, 화합물

생성물 1

HCID 178445900HCID 178445900, 화합물

시약·촉매·용매 2

HCID 6228
Dimethylformamide
용매
HCID 8471Triethylamine용매

실험 절차

To a solution of 190 mg of (±)-2-(1-naphthylmethyl)-5-phenyl-4-pentenoic acid and 400 mg of bis(P-toluenesulfonic acid) salt of L-histidyl-L-leucinal semicarbazone in 7 ml of N,N-dimethylformamide were successively added 0.16 ml of diphenylphosphoryl azide and 0.28 ml of triethylamine under ice-cooling, and the mixture was stirred overnight. To the reaction mixture was added a 5% aqueous sodium bicarbonate solution, and the mixture was extracted withh ethyl acetate and washed with water. The organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel flash column chromatography (eluent: chloroform/methanol=15/1 by volume) to obtain 151 mg of N-[(±)-2-(1-naphthylmethyl)-5-phenyl-4-pentenoyl]-L-histidyl-L-leucinal semicarbazone as a white powder.

후처리

  1. temperaturecooling
  2. extractionthe mixture was extracted withh ethyl acetate
  3. washwashed with water
  4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel flash column chromatography (eluent: chloroform/methanol=15/1 by volume)

출처 및 근거

ORD 기록
ord-c7a7a68bbcd7411991d531ef0d1bc376
출처 데이터셋
uspto-grants-1989_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04863904

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