Triethylamine → 2-(2-Isopropyl-1,3-dioxolan-2-yl)ethyl methanesulfonate

HRID 80980ノート

反応式

HRID 80980 の反応式
[CH:1]([C:4]1([CH2:9][CH2:10][OH:11])[O:8][CH2:7][CH2:6][O:5]1)([CH3:3])[CH3:2].C(N(CC)CC)C.[CH3:19][S:20](Cl)(=[O:22])=[O:21]>C(Cl)Cl>[CH:1]([C:4]1([CH2:9][CH2:10][O:11][S:20]([CH3:19])(=[O:22])=[O:21])[O:8][CH2:7][CH2:6][O:5]1)([CH3:3])[CH3:2]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 141623372-[2-(Propan-2-yl)-1,3-dioxolan-2-yl]ethan-1-ol

生成物 1

HCID 107051032-(2-Isopropyl-1,3-dioxolan-2-yl)ethyl methanesulfonate収率 100.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2-(2-isopropyl-1,3-dioxolan-2-yl)-ethanol (8.0 g, 50 mmol) and triethylamine (23.5 mL, 170 mmol) in anhydrous CH2Cl2 (120 mL) was added methanesulfonyl chloride (11.6 mL, 150 mmol) at 0° C., and the reaction mixture was stirred at room temperature till the reaction was finished. The reaction mixture was washed with water and brine, dried over Na2SO4, filtered, and concentrated to give the crude methanesulfonic acid 2-(2-isopropyl-[1,3]dioxolan-2-yl)-ethyl ester (12 g), which was used for the next step without further purification.

後処理

  1. washThe reaction mixture was washed with water and brine
  2. dry with materialdried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-1a15484b2a5546a3a8afc2433a8478aa
出典データセット
uspto-grants-2014_09
特許番号
US08846668B2

反応ノート

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