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Hydrazine hydrate (1:1) → 4-(1-Hydroxyethyl)pyrazolidin-3-one

HRID 1029668
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HRID 1029668 반응식
O.[NH2:2][NH2:3].[OH:4][CH:5]([C:7](=[CH2:13])[C:8](OCC)=[O:9])[CH3:6]>C(O)C>[OH:4][CH:5]([CH:7]1[CH2:13][NH:3][NH:2][C:8]1=[O:9])[CH3:6]
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 10855587Butanoic acid, 3-hydroxy-2-methylene-, ethyl ester

생성물 1

HCID 143142834-(1-Hydroxyethyl)pyrazolidin-3-one수율 71.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To hydrazine hydrate (38.6 g) was added dropwise a solution of ethyl 2-(1-hydroxyethyl)acrylate (106 g) in ethanol (20 ml) at 0° C. After the addition, the reaction mixture was allowed to warm to room temperature and stirred for 4 hours at the same temperature. The resulting reaction mixture was chromatographed on silica gel (2.2 l) eluting in turn with chloroform and a mixture of chloroform and methanol (8:1→2:1→1:1, V/V) to give 4-(1-hydroxyethyl)-3-pyrazolidinone (68 g).

후처리

  1. additionAfter the addition
  2. customThe resulting reaction mixture
  3. customwas chromatographed on silica gel (2.2 l)
  4. washeluting in turn with chloroform
  5. additiona mixture of chloroform and methanol (8:1→2:1→1:1, V/V)

출처 및 근거

ORD 기록
ord-f1171f2b3ef34aa3a0358caba1e01006
출처 데이터셋
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05102877

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