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Hydrazine hydrate (1:1) → 1-Ethyl-3-(7-hydrazinocarbonyl-5-pyridin-3-yl-benzothiazol-2-yl)-urea

HRID 447032
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HRID 447032 반응식
C[O:2][C:3]([C:5]1[C:13]2[S:12][C:11]([NH:14][C:15]([NH:17][CH2:18][CH3:19])=[O:16])=[N:10][C:9]=2[CH:8]=[C:7]([C:20]2[CH:21]=[N:22][CH:23]=[CH:24][CH:25]=2)[CH:6]=1)=O.O.[NH2:27][NH2:28]>CO.O>[CH2:18]([NH:17][C:15]([NH:14][C:11]1[S:12][C:13]2[C:5]([C:3]([NH:27][NH2:28])=[O:2])=[CH:6][C:7]([C:20]3[CH:21]=[N:22][CH:23]=[CH:24][CH:25]=3)=[CH:8][C:9]=2[N:10]=1)=[O:16])[CH3:19]
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참가 물질

5

반응물 2

HCID 24654Hydrazine hydrate (1:1)2회HCID 578136192-(3-Ethyl-ureido)-5-pyridin-3-yl-benzothiazole-7-carboxylic acid methyl ester

생성물 1

HCID 578136141-Ethyl-3-(7-hydrazinocarbonyl-5-pyridin-3-yl-benzothiazol-2-yl)-urea수율 98%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

A suspension of 2-(3-Ethyl-ureido)-5-pyridin-3-yl-benzothiazole-7-carboxylic acid methyl ester (319 mg, 0.895 mmol) in methanol (10 ml) was treated with hydrazine hydrate (2 ml) and stirred at ambient temperature for 16 h. HPLC indicated that the reaction mixture still contained a considerable amount of starter so a further 1 ml of hydrazine hydrate was added and the stirring continued for a further 24 h. The resultant mixture was diluted with water (50 ml) and the solid collected by filtration. This was washed with water (25 ml) followed by ethanol (25 ml) and dried in vacuo to give 1-Ethyl-3-(7-hydrazinocarbonyl-5-pyridin-3-yl-benzothiazol-2-yl)-urea as an off-white solid (312 mg, 98%).

후처리

  1. additionwas added
  2. waitthe stirring continued for a further 24 h
  3. filtrationthe solid collected by filtration
  4. washThis was washed with water (25 ml)
  5. customdried in vacuo

출처 및 근거

ORD 기록
ord-da4456fa5b34460096490ac104f001af
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08481544B2

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