Triethylamine → 2-(2-Fluorophenyl)ethyl methanesulfonate

HRID 1992397

반응식

HRID 1992397 반응식
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][CH2:9][OH:10].C(N(CC)CC)C.[CH3:18][S:19](Cl)(=[O:21])=[O:20]>ClCCl>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][CH2:9][O:10][S:19]([CH3:18])(=[O:21])=[O:20]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 27332962-(2-Fluorophenyl)ethan-1-ol

생성물 1

HCID 151245352-(2-Fluorophenyl)ethyl methanesulfonate수율 94.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 2-(2-fluorophenyl)-ethanol (4.00 g, 28.5 mmol) and triethylamine (6.36 mL, 45.7 mmol) in dichloromethane (15 mL) was added methanesulfonyl chloride (2.88 mL, 37.1 mmol) at −5° C. The mixture was stirred for 4 hours and was allowed to slowly warm to room temperature. The mixture was diluted with dichloromethane and extracted with 1 M HCl and water. The organic layer was dried over Na2SO4 and concentrated in vacuo. The crude product was purified by column chromatography, using dichloromethane as eluent, to afford 5.88 g (94.4%) the title compound.

후처리

  1. extractionextracted with 1 M HCl and water
  2. dry with materialThe organic layer was dried over Na2SO4
  3. concentrationconcentrated in vacuo
  4. customThe crude product was purified by column chromatography

출처 및 근거

ORD 기록
ord-15f8a62e0fe24d1bac4f43f7d4add78f
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07648985B2

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