Solketal → (2,2-Dimethyl-1,3-dioxolan-4-yl)methyl methanesulfonate

温度

0 °C

To a solution of (2,2-dimethyl-[1,3]dioxolan-4-yl)-methanol (1.25 g, 9.46 mmol) and triethylamine (9.2 ml, 66.2 mmol) in dichloromethane (60 ml) at 0° C. was slowly added methanesulfonyl chloride (2.2 ml, 28.4 mmol). The reaction mixture was stirred at 0° C. for 2 h then quenched with water and the aqueous layer was extracted with dichloromethane. The combined organics were washed with 10% citric acid, sat NaHCO3, and brine then dried over MgSO4 and concentrated to afford methanesulfonic acid 2,2-dimethyl-[1,3]dioxolan-4-ylmethyl ester as a light brown oil which was used without further purification.

1. customat 0° C.
2. customthen quenched with water
3. extractionthe aqueous layer was extracted with dichloromethane
4. washThe combined organics were washed with 10% citric acid
5. dry with materialthen dried over MgSO4
6. concentrationconcentrated

ORDレコード

ord-402d486a81b84fbaa9544902b15926cb

出典データセット

uspto-grants-2014_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08658646B2