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2-Bromoethanol → 2-(4-(Methylsulfonyl)piperidin-1-yl)ethanol

HRID 85732
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인쇄 미리보기

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HRID 85732 반응식
Cl.[CH3:2][S:3]([CH:6]1[CH2:11][CH2:10][NH:9][CH2:8][CH2:7]1)(=[O:5])=[O:4].Br[CH2:13][CH2:14][OH:15].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH3:2][S:3]([CH:6]1[CH2:11][CH2:10][N:9]([CH2:13][CH2:14][OH:15])[CH2:8][CH2:7]1)(=[O:5])=[O:4]
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참가 물질

5

반응물 3

HCID 108982-BromoethanolHCID 11430Potassium CarbonateHCID 230616984-Methanesulfonylpiperidine hydrochloride

생성물 1

HCID 682760202-(4-(Methylsulfonyl)piperidin-1-yl)ethanol수율 66.3%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
60 °C

실험 절차

A mixture of 4-(methylsulfonyl)piperidine hydrochloride (900 mg, 4.51 mmol), 2-bromoethanol (1126 mg, 9.01 mmol) and potassium carbonate (1869 mg, 13.52 mmol) in acetonitrile (4 mL) was heated up at 60° C. for 13 hours. The reaction mixture was cooled to room temperature and concentrated under reduced pressure to provide the crude, the crude was purified by 0-35% ethyl acetate/methanol to provide the desired product as colorless oil (620 mg, 66%). LCMS: m/e 208.1 (M+H)+, 0.27 min (method 6).

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. concentrationconcentrated under reduced pressure
  3. customto provide the crude
  4. customthe crude was purified by 0-35% ethyl acetate/methanol

출처 및 근거

ORD 기록
ord-ae007d14b87c49fcbc10dce9ad81f20d
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08846647B2

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