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7-Chloro-2-hydrazinyl-5-phenyl-3H-1,4-benzodiazepine → HCID 53749252、化合物

HRID 328386
ノート
印刷プレビュー

反応式

HRID 328386 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]=[C:10]([NH:12][NH2:13])[CH2:9][N:8]=[C:7]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:6]=2[CH:20]=1.Cl.[CH2:22]([N:24]([CH2:33][CH3:34])[CH2:25][CH2:26][CH2:27][C:28](=O)[C:29]([OH:31])=[O:30])[CH3:23]>CO>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]=[C:10]([NH:12][N:13]=[C:28]([C:29]([OH:31])=[O:30])[CH2:27][CH2:26][CH2:25][N:24]([CH2:33][CH3:34])[CH2:22][CH3:23])[CH2:9][N:8]=[C:7]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:6]=2[CH:20]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 123908747-Chloro-2-hydrazinyl-5-phenyl-3H-1,4-benzodiazepineHCID 131710708HCID 131710708、化合物

生成物 1

HCID 53749252HCID 53749252、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a stirred solution of 2.85 g. (0.01 mole) of 7-chloro-2-hydrazino-5-phenyl-3H-1,4-benzodiazepine in 100 ml. of methanol is added 2.24 g. (0.01 mole) of 5-(diethylamino)-2-oxo-valeric acid, hydrochloride [prepared by the method of Libman and Kutznetsov J. Gen. Chem. (USSR), 33, 1938 (1963)]. The mixture is kept under nitrogen at ambient temperature for 2 hours and then concentrated in vacuo. The residue is mixed with aqueous sodium bicarbonate and extracted with methylene chloride. The extract was washed with brine, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue of 7-chloro-2-[[1-carboxy-4-(diethylamino)-butylidene]hydrazino]-5-phenyl-3H-1,4-benzodiazepine is used without further purification.

後処理

  1. concentrationconcentrated in vacuo
  2. additionThe residue is mixed with aqueous sodium bicarbonate
  3. extractionextracted with methylene chloride
  4. washThe extract was washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe residue of 7-chloro-2-[[1-carboxy-4-(diethylamino)-butylidene]hydrazino]-5-phenyl-3H-1,4-benzodiazepine is used without further purification

出典と根拠

ORDレコード
ord-6c64648af2104185bb082a2f0ef3b944
出典データセット
uspto-grants-1977_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04017492

反応ノート

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