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Hydrazine hydrate (1:1) → N-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenyl)-5-oxopyrazolidine-3-carboxamide

HRID 1641451
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HRID 1641451 반응식
O.[NH2:2][NH2:3].[Cl:4][C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12](=[O:19])/[CH:13]=[CH:14]\[C:15](OC)=[O:16])=[C:7]([C:20](=[O:27])[NH:21][CH:22]([CH:24]2[CH2:26][CH2:25]2)[CH3:23])[CH:6]=1>C(O)C>[Cl:4][C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12]([CH:13]2[CH2:14][C:15](=[O:16])[NH:3][NH:2]2)=[O:19])=[C:7]([C:20](=[O:27])[NH:21][CH:22]([CH:24]2[CH2:26][CH2:25]2)[CH3:23])[CH:6]=1
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 66737717Methyl 4-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenylamino)-4-oxoisocrotonate

생성물 1

HCID 44185604N-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenyl)-5-oxopyrazolidine-3-carboxamide수율 52%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

3.58 g of hydrazine monohydrate was dropwise added to a mixed liquid comprising 25 g of methyl 4-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenylamino)-4-oxoisocrotonate and 250 ml of ethanol, followed by reflux with heating. After stirring for 5.5 hours, the reaction liquid was stood to cool. The precipitated crystals were subjected to suction filtration. The crystals collected after the filtration were washed with ethyl acetate and then with hexane and air dried to obtain 13 g of the desired product.

후처리

  1. temperatureby reflux
  2. temperaturewith heating
  3. customthe reaction liquid
  4. temperatureto cool
  5. filtrationThe precipitated crystals were subjected to suction filtration
  6. customThe crystals collected
  7. filtrationafter the filtration
  8. washwere washed with ethyl acetate
  9. dry with materialwith hexane and air dried

출처 및 근거

ORD 기록
ord-32985c6815b94f4b9c062ea26e2d8738
출처 데이터셋
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08115006B2

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