Water → 2-Cyclopropylethyl methanesulfonate

To a solution of 2-cyclopropylethanol (2.1 g, 24.4 mmol) in dichloromethane (50 ml) at 0° C. under nitrogen was added triethylamine (4.1 ml, 1.2 mol. equiv.). Methanesulphonyl chloride (2.5 ml, 1.3 mol. equiv.) was added, dropwise, and the reaction allowed to stir for 18 hours at room temperature. Water (50 ml) and dichloromethane (50 ml) were added. The organic phase was separated, washed with water (2×50 ml) and then dried over anhydrous sodium sulphate. The solution was filtered and the solvent removed from the filtrate by evaporation under reduced pressure to give the title compound as an oil (4 g). TLC Rf=0.9 (silica, methanol:dichloromethane, 1:19, by volume). LRMS m/z=182 (m+18)+.

1. customThe organic phase was separated
2. washwashed with water (2×50 ml)
3. dry with materialdried over anhydrous sodium sulphate
4. filtrationThe solution was filtered
5. customthe solvent removed from the filtrate by evaporation under reduced pressure

ORDレコード

ord-ecfd5f27621649f6ba2ed88a7ea7819e

出典データセット

uspto-grants-2001_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06262075B1