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Ethyl Glycolate → 2-Hydroxy-1-(4-methylpiperazin-1-yl)ethan-1-one

HRID 1051784
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인쇄 미리보기

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HRID 1051784 반응식
[OH:1][CH2:2][C:3]([O:5]CC)=O.[CH3:8][N:9]1[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1>O1CCOCC1>[OH:1][CH2:2][C:3]([N:12]1[CH2:13][CH2:14][N:9]([CH3:8])[CH2:10][CH2:11]1)=[O:5]
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참가 물질

4

반응물 2

HCID 12184Ethyl GlycolateHCID 531671-Methylpiperazine

생성물 1

HCID 150689652-Hydroxy-1-(4-methylpiperazin-1-yl)ethan-1-one

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
120 °C

실험 절차

Ethyl 2-hydroxyacetate (6.85 g, 65.8 mmol, 1.0 eq) and 1-methylpiperazine (5.26 g, 52.6 mmol, 0.8 eq) were dissolved in 1,4-dioxane (10 mL) in a sealed tube and the mixture was stirred at 120° C. overnight. The mixture was allowed to cool to RT and then concentrated in vacuo. The residue was purified by flash column chromatography on silica gel (2% MeOH-DCM) to afford the product 2-hydroxy-1-(4-methyl piperazin-1-yl)ethanone.

후처리

  1. temperatureto cool to RT
  2. concentrationconcentrated in vacuo
  3. customThe residue was purified by flash column chromatography on silica gel (2% MeOH-DCM)

출처 및 근거

ORD 기록
ord-2ec1ae13a61e4ecea1ce941a20a54b4e
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09388183B2

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