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

HRID 470428ノート

反応式

HRID 470428 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>[CH3:19][S:20]([O:11][CH2:10][CH2:9][C:4]1([CH:1]([CH3:3])[CH3:2])[O:8][CH2:7][CH2:6][O:5]1)(=[O:22])=[O:21]

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 rt till the reaction was finished. The reaction mixture was washed with water and brine, dried over Na2SO4, filtered, and concentrated to give the crude 2-(2-isopropyl-1,3-dioxolan-2-yl)ethyl methanesulfonate (12 g, crude), 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-bd97f5993da24a44a77147c8cb9c78d6
出典データセット
uspto-grants-2014_01
特許番号
US08629138B2

反応ノート

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