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Acetic Anhydride → (S)-4-Acetyl-2-piperazinemethanol

HRID 1196874
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HRID 1196874 반응식
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][C@H:2]1[CH2:7][OH:8].[C:9](OC(=O)C)(=[O:11])[CH3:10].C(=O)([O-])[O-].[Na+].[Na+]>O.C(N(CC)CC)C>[NH3:1].[C:9]([N:4]1[CH2:5][CH2:6][NH:1][C@H:2]([CH2:7][OH:8])[CH2:3]1)(=[O:11])[CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 7918Acetic AnhydrideHCID 10340Sodium CarbonateHCID 14288866[(2S)-piperazin-2-yl]methanol

생성물 2

HCID 222AmmoniaHCID 45086134(S)-4-Acetyl-2-piperazinemethanol수율 287.3%

시약·촉매·용매 2

HCID 962Water용매2회HCID 8471Triethylamine

실험 절차

A solution of (S)-2-piperazinemethanol (1.25 g) in a mixture of water (12 ml) and triethylamine (3.2 ml) at ambient temperature was treated with a solution of acetic anhydride (1.25 ml; 1.32 mmol) in water (25 ml). The mixture was stirred at ambient temperature for 1 h, and anhydrous sodium carbonate (2 g) was added. The solvent was removed in vacuo. The residue was purified by flash column chromatography using dichloromethane:methanol:ammonia, 75:10:2 as eluant to give the title compound as a pale yellow oil (0.6 g).

후처리

  1. customThe solvent was removed in vacuo
  2. customThe residue was purified by flash column chromatography

출처 및 근거

ORD 기록
ord-87fb5d5dabe04b9784a6cdd10cc24fab
출처 데이터셋
uspto-grants-1992_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05116842

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