反応式
[Cl:1][CH2:2][CH2:3][O:4][CH2:5][CH2:6][OH:7].C(N(CC)CC)C.[CH3:15][S:16](Cl)(=[O:18])=[O:17].O>C1(C)C=CC=CC=1>[S:16]([O:7][CH2:6][CH2:5][O:4][CH2:3][CH2:2][Cl:1])(=[O:18])(=[O:17])[CH3:15]参加物
6
反応条件
- 温度
- 5 °C
実験手順
To a solution of 2-(2-chloroethoxy)ethanol (15.3 g, 123 mmol) in toluene (100 ml) kept at 5° C. was added triethylamine (50 g, 500 mmol). A solution of methanesulfonyl chloride (28 g, 245 mmol) in toluene (50 ml) was carefully added keeping the temperature around 5° C. When addition was complete the reaction mixture was stirred at 5° C. for 45 minutes and then 75 minutes at ambient temperature. Water (100 ml) was added and the mixture was stirred for 15 minutes. The phases were separated and the organic phase was washed with water, brine and dried over magnesium sulphate. The solvent was evaporated in vacuo to give crude 2-(2-chloroethoxy)ethyl mesylate as an oil.
後処理
- customkept at 5° C.
- customthe temperature around 5° C
- additionWhen addition
- custom75 minutes
- customat ambient temperature
- stirringthe mixture was stirred for 15 minutes
- customThe phases were separated
- washthe organic phase was washed with water, brine
- dry with materialdried over magnesium sulphate
- customThe solvent was evaporated in vacuo
出典と根拠
- ORDレコード
- ord-109ceabd173a4a51882d63eb6799949d
- 出典データセット
- uspto-grants-1994_09
- 特許番号
- US05348965
関連ノート
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