2-Chlorocyclohexanone → HCID 23312424、化合物

HRID 745756ノート

反応式

HRID 745756 の反応式
Cl.N[C:3]1CC[N:5]([C:8]2[S:9][C:10]3[CH2:16][CH2:15][CH2:14][CH2:13][C:11]=3[N:12]=2)[N:4]=1.C(NNC(N)=S)=[O:18].[Cl:24]C1CCCCC1=O>CN(C)C=O>[ClH:24].[CH:3]([NH:4][NH:5][C:8]1[S:9][C:10]2[CH2:16][CH2:15][CH2:14][CH2:13][C:11]=2[N:12]=1)=[O:18]

参加物

5

反応物 3

HCID 132032-ChlorocyclohexanoneHCID 27754861-Formyl-3-thiosemicarbazideHCID 23312414HCID 23312414、化合物

生成物 1

HCID 23312424HCID 23312424、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

The 2-hydrazino-4,5,6,7-tetrahydro-benzothiazole hydrochloride used above is prepared in accordance with the method of Y.Usui [CA 70,96685 (1969)] via Hantzsch synthesis, with better yields by modification of the conditions. A mixture of 20 g of formylthiosemicarbazide, 22.3 g of 2-chlorocyclohexanone and 150 ml of dimethylformamide is kept at 70°-80° C. for 3 hours. On cooling, some of the product crystallises out. The dimethylformamide is distilled off in vacuo and the residue is recrystallised from ethanol. 27.4 g of 1-formyl-2-(4,5,6,7-tetrahydro-benzothiazolyl)-hydrazine hydrochloride of melting point 171°-173° C. are obtained.

後処理

  1. customabove is prepared in accordance with the method of Y.Usui [CA 70,96685 (1969)] via Hantzsch synthesis
  2. customwith better yields by modification of the conditions
  3. temperatureOn cooling
  4. customsome of the product crystallises out
  5. distillationThe dimethylformamide is distilled off in vacuo
  6. customthe residue is recrystallised from ethanol

出典と根拠

ORDレコード
ord-85e79c7c84a14e198a5d9b7ae9deefdc
出典データセット
uspto-grants-1986_07
特許番号
US04600722

反応ノート

読み込み中…