Triphenylphosphine → 2-ethoxy-7-nitro-5-phenyl-3H-1,4-benzodiazepine

HRID 867061노트

반응식

HRID 867061 반응식
[N:1]([CH2:4][C:5](=[N:9][C:10]1[CH:23]=[CH:22][C:21]([N+:24]([O-:26])=[O:25])=[CH:20][C:11]=1[C:12]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)=O)[O:6][CH2:7][CH3:8])=[N+]=[N-].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C1C=CC=CC=1>[CH2:7]([O:6][C:5]1[CH2:4][N:1]=[C:12]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:11]2[CH:20]=[C:21]([N+:24]([O-:26])=[O:25])[CH:22]=[CH:23][C:10]=2[N:9]=1)[CH3:8]

참가 물질

4

반응물 2

HCID 11776TriphenylphosphineHCID 203172632-(2-Azido-1-ethoxyethylideneamino)-5-nitrobenzophenone

생성물 1

HCID 203172642-ethoxy-7-nitro-5-phenyl-3H-1,4-benzodiazepine

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

To a solution of 2.5 parts of 2-(2-azido-1-ethoxyethylideneamino)-5-nitrobenzophenone produced in Step (2) in 30 parts by volume of benzene is added with stirring 1.78 parts of triphenylphosphine. The mixture is stirred for further 1.5 hours and the solvent is removed by distillation. The residue is extracted with a mixture of n-hexane and acetone (7:3), and the soluble fraction is purified by means of chromatography employing Silica Gel, whereupon 2-ethoxy-7-nitro-5-phenyl-3H-1,4-benzodiazepine is obtained as pale yellow crystals. Recrystallization from ether-n-hexane gives pale yellow prisms melting at 143°-145° C.

후처리

  1. customthe solvent is removed by distillation
  2. extractionThe residue is extracted with a mixture of n-hexane and acetone (7:3)
  3. customthe soluble fraction is purified by means of chromatography

출처 및 근거

ORD 기록
ord-e605eaf53e8a4d72bd3be540b5d972d5
출처 데이터셋
uspto-grants-1978_07
특허 번호
US04102881

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