HCID 21317692、化合物 → Fluclotizolam

HRID 262976ノート

反応式

HRID 262976 の反応式
[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

参加物

3

反応物 1

HCID 21317692HCID 21317692、化合物

生成物 1

HCID 21317700Fluclotizolam

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-705bf0a3a623430d9df117106fb0cbe8
出典データセット
uspto-grants-1979_05
特許番号
US04155913

反応ノート

読み込み中…