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

HRID 85732ノート

反応式

HRID 85732 の反応式
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]

参加物

5

反応物 3

HCID 108982-BromoethanolHCID 11430Potassium CarbonateHCID 230616984-Methanesulfonylpiperidine hydrochloride

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
60 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-ae007d14b87c49fcbc10dce9ad81f20d
出典データセット
uspto-grants-2014_09
特許番号
US08846647B2

反応ノート

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