2-Hydroxyacetohydrazide → 2-chloro-4-(o-chlorophenyl)-6H-thieno[3,2-f]-s-triazolo[4,3-a][1,4]diazepine-9-methanol

HRID 262986

反応式

HRID 262986 の反応式
[Cl:1][C:2]1[S:19][C:5]2[NH:6][C:7](=S)[CH2:8][N:9]=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[Cl:17])[C:4]=2[CH:3]=1.[C:20]([NH:24][NH2:25])(=O)[CH2:21][OH:22]>C(O)CCC>[Cl:1][C:2]1[S:19][C:5]2[N:6]3[C:20]([CH2:21][OH:22])=[N:24][N:25]=[C:7]3[CH2:8][N:9]=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[Cl:17])[C:4]=2[CH:3]=1

参加物

4

反応物 2

HCID 3505362-HydroxyacetohydrazideHCID 1357830787-Chloro-5-(2-chlorophenyl)-1,3-dihydro-2H-thieno-(2,3-e)-(1,4)-diazepine-2-thione

生成物 1

HCID 213176872-chloro-4-(o-chlorophenyl)-6H-thieno[3,2-f]-s-triazolo[4,3-a][1,4]diazepine-9-methanol

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

1.1 g of 7-chloro-5-(o-chlorophenyl)-1,3-dihydro-2H-thieno[2,3-e]-1,4-diazepine-2-thione are refluxed for 8 hours with 1.5 g of glycolic acid hydrazide in absolute butanol. The solvent is then distilled off and the residue recrystallized from ethyl acetate containing active carbon to yield 2-chloro-4-(o-chlorophenyl)-6H-thieno[3,2-f]-s-triazolo[4,3-a][1,4]diazepine-9-methanol, melting point 219°-221° C.

後処理

  1. distillationThe solvent is then distilled off
  2. customthe residue recrystallized from ethyl acetate containing active carbon

出典と根拠

ORDレコード
ord-9309f7b55c5046fc9ce40bf1bacba5b2
出典データセット
uspto-grants-1979_05
特許番号
US04155913

関連ノート

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