2-Chlorocyclohexanone → HCID 23312424, 화합물

HRID 745756노트

반응식

HRID 745756 반응식
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]

참가 물질

5

반응물 3

HCID 132032-ChlorocyclohexanoneHCID 27754861-Formyl-3-thiosemicarbazideHCID 23312414HCID 23312414, 화합물

생성물 1

HCID 23312424HCID 23312424, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-85e79c7c84a14e198a5d9b7ae9deefdc
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04600722

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