Water → 3-Fluoropropyl methanesulfonate

To an ice cold, stirred solution of 19.0 g (0.244 mole) of 3-fluoropropanol and 39.5 g (0.300 mole) of triethylamine in 300 mL of methylene chloride was added dropwise 34.4 g (0.300 mole) of methanesulfonyl chloride. The resultant mixture was allowed to warm to room temperature and was stirred for approximately 18 hours. The mixture was poured into water and was washed with an aqueous, saturated sodium bicarbonate solution. The organic phase was dried over anhydrous magnesium sulfate and was filtered. The filtrate was distilled under reduced pressure to yield 41.3 g of 3-fluoropropyl methanesulfonate as a liquid, bp 116° C./15 mm Hg.

1. washwas washed with an aqueous, saturated sodium bicarbonate solution
2. dry with materialThe organic phase was dried over anhydrous magnesium sulfate
3. filtrationwas filtered
4. distillationThe filtrate was distilled under reduced pressure

ORDレコード

ord-d0d60b880939475fb91ef69a1ac6be78

出典データセット

uspto-grants-1991_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05035740