2-Phenylethanol → Methanesulfonic acid, 2-phenylethyl ester

HRID 1773860ノート

反応式

HRID 1773860 の反応式
[C:1]1([CH2:7][CH2:8][OH:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CCN(CC)CC.[CH3:17][S:18](Cl)(=[O:20])=[O:19]>C(Cl)Cl>[CH2:8]([O:9][S:18]([CH3:17])(=[O:20])=[O:19])[CH2:7][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

5

反応物 3

HCID 60542-PhenylethanolHCID 8471TriethylamineHCID 31297Methanesulfonyl chloride

生成物 1

HCID 146679Methanesulfonic acid, 2-phenylethyl ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

To a solution of 2-phenylethanol (24.4 g, 0.2 mole) in CH2Cl2 (200 mL) is added NEt3 (30.7 mL, 0.22 mole). The reaction mixture is cooled to 0° C. and methanesulfonyl chloride (16.3 mL, 0.21 mole) is added dropwise. The reaction mixture is allowed to reach room temperature and is stirred at room temperature overnight. Solvent is removed under reduced pressure. Water is added and the aqueous phase is extracted three times with Et2O. The organic phase is washed with water, brine, dried over magnesium sulphate, filtered and the solvent is removed under reduced pressure to give methanesulfonic acid phenethyl ester.

後処理

  1. customto reach room temperature
  2. customSolvent is removed under reduced pressure
  3. additionWater is added
  4. extractionthe aqueous phase is extracted three times with Et2O
  5. washThe organic phase is washed with water, brine
  6. dry with materialdried over magnesium sulphate
  7. filtrationfiltered
  8. customthe solvent is removed under reduced pressure

出典と根拠

ORDレコード
ord-d6910f16b73e49cd9e87621c1a070bb6
出典データセット
uspto-grants-2016_02
特許番号
US09255101B2

反応ノート

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