Triethylamine → 2-(2-Fluorophenyl)ethyl methanesulfonate

HRID 1992397

反応式

HRID 1992397 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 151245352-(2-Fluorophenyl)ethyl methanesulfonate収率 94.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-15f8a62e0fe24d1bac4f43f7d4add78f
出典データセット
uspto-grants-2010_01
特許番号
US07648985B2

関連ノート

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