HCID 21317692, 화합물 → Fluclotizolam

HRID 262976노트

반응식

HRID 262976 반응식
[C:1]([NH:4][NH:5][C:6]1[CH2:7][N:8]=[C:9]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=2[F:23])[C:10]2[CH:15]=[C:14]([Cl:16])[S:13][C:11]=2[N:12]=1)(=O)[CH3:2]>C1(C)C(C)=CC=CC=1>[Cl:16][C:14]1[S:13][C:11]2[N:12]3[C:1]([CH3:2])=[N:4][N:5]=[C:6]3[CH2:7][N:8]=[C:9]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[F:23])[C:10]=2[CH:15]=1

참가 물질

3

반응물 1

HCID 21317692HCID 21317692, 화합물

생성물 1

HCID 21317700Fluclotizolam

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

6.8 g of 2-(2-acetylhydrazino)-7-chloro-5-(o-fluorophenyl)-3H-thieno[2,3-e]-1,4-diazepine are refluxed for 9 hours in 300 ml of absolute xylene. After cooling, the precipitated impurities are filtered off under vacuum. The solvent is then evaporated under reduced pressure and the product recrystallized from ethyl acetate containing active carbon to yield 2-chloro-4-(o-fluorophenyl)-9-methyl-6H-thieno[3,2-f]-s-triazolo[4,3-a][1,4]diazepine, melting point 187°-189° C.

후처리

  1. temperatureAfter cooling
  2. filtrationthe precipitated impurities are filtered off under vacuum
  3. customThe solvent is then evaporated under reduced pressure
  4. customthe product recrystallized from ethyl acetate containing active carbon

출처 및 근거

ORD 기록
ord-705bf0a3a623430d9df117106fb0cbe8
출처 데이터셋
uspto-grants-1979_05
특허 번호
US04155913

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