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2-Bromoethanol → (R)-2-(4-acetyl-3-methylpiperazin-1-yl)ethanol

HRID 2381143
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HRID 2381143 반응식
Br[CH2:2][CH2:3][OH:4].[C:5]([N:8]1[CH2:13][CH2:12][NH:11][CH2:10][C@H:9]1[CH3:14])(=[O:7])[CH3:6].C(=O)([O-])[O-].[K+].[K+]>C1COCC1>[C:5]([N:8]1[CH2:13][CH2:12][N:11]([CH2:2][CH2:3][OH:4])[CH2:10][C@H:9]1[CH3:14])(=[O:7])[CH3:6]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 108982-BromoethanolHCID 11430Potassium CarbonateHCID 55300442(R)-1-(2-Methylpiperazin-1-YL)ethanone

생성물 1

HCID 68499640(R)-2-(4-acetyl-3-methylpiperazin-1-yl)ethanol수율 97.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
80 °C
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실험 절차

2-Bromoethanol (7.34 mL, 103.38 mmol) was added to a stirred mixture of (R)-1-acetyl-2-methylpiperazine (2.94 g, 20.68 mmol) and potassium carbonate (8.57 g, 62.03 mmol) in THF (75 mL). The resulting mixture was stirred at 80° C. for 18 hours before, then filtered and evaporated. The residue was purified by ion exchange chromatography, using an SCX column and eluting with 2M ammonia in methanol. Pure fractions were evaporated to dryness to give (R)-2-(4-acetyl-3-methylpiperazin-1-yl)ethanol (3.74 g, 97%) as a yellow oil.

후처리

  1. filtrationthen filtered
  2. customevaporated
  3. customThe residue was purified by ion exchange chromatography
  4. washeluting with 2M ammonia in methanol
  5. customPure fractions were evaporated to dryness

출처 및 근거

ORD 기록
ord-490d7fb2983b416590b5ac7b4f06cadd
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08258140B2

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