三乙胺 → 2-(2-Isopropyl-1,3-dioxolan-2-yl)ethyl methanesulfonate

HRID 80980笔记

反应方程式

HRID 80980 反应方程式
[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]

参与物

5

反应物 3

HCID 8471三乙胺HCID 31297甲基磺酰氯HCID 141623372-[2-(Propan-2-yl)-1,3-dioxolan-2-yl]ethan-1-ol

产物 1

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

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂

实验过程

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.

后处理

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

来源与证据

ORD记录
ord-1a15484b2a5546a3a8afc2433a8478aa
来源数据集
uspto-grants-2014_09
专利号
US08846668B2

反应笔记

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