2-Methylimidazole → Estazolam

HRID 1764513

반응식

HRID 1764513 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 3261Estazolam

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2f9d688256f6492a8e3493b7ddfa1c2a
출처 데이터셋
uspto-grants-1978_09
특허 번호
US04116956

연결된 노트

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