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

HRID 867061ノート

反応式

HRID 867061 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e605eaf53e8a4d72bd3be540b5d972d5
出典データセット
uspto-grants-1978_07
特許番号
US04102881

反応ノート

読み込み中…