2-Methylimidazole → Estazolam

HRID 1764513

反応式

HRID 1764513 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.[CH:22](N)=N.CC1NC=CN=1>O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[CH:22]=[N:13][N:12]=[C:10]3[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

5

反応物 3

HCID 127492-MethylimidazoleHCID 10313058Methanimidamide, hydrochloride (1:1)HCID 123908747-Chloro-2-hydrazinyl-5-phenyl-3H-1,4-benzodiazepine

生成物 1

HCID 3261Estazolam

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 2.8 parts of 7-chloro-2-hydrazino-5-phenyl-3H-1,4-benzodiazepine, 2.4 parts of formamidine hydrochloride and 2.5 parts of 2-methylimidazole is fused at 160° C for 10 minutes. Water is added to the mixture, followed by extraction with methylene chloride. The methylene chloride layer is washed with water, dried over sodium sulfate and the solvent is evaporated, whereby 8-chloro-6-phenyl-4H-s-triazolo [4,3-a][1,4] benzodiazepine is yielded. Recrystallization from ethyl acetate yields colorless flakes melting at 226° C to 227° C.

後処理

  1. extractionfollowed by extraction with methylene chloride
  2. washThe methylene chloride layer is washed with water
  3. dry with materialdried over sodium sulfate
  4. customthe solvent is evaporated

出典と根拠

ORDレコード
ord-2f9d688256f6492a8e3493b7ddfa1c2a
出典データセット
uspto-grants-1978_09
特許番号
US04116956

関連ノート

読み込み中…