Chlorosulfonic acid → 4-((R)-2-Fluoro-1-methyl-ethyl)-benzenesulfonyl chloride

温度

2.5 °C

1.3 g of ((R)-2-fluoro-1-methyl-ethyl)-benzene (9.4 mmol) were dissolved in 50 ml of dichloromethane. At 0-5° C., 1.1 g of chlorosulfonic acid (9.4 mmol), dissolved in 10 ml of dichloromethane, were added dropwise. The reaction mixture was stirred for 20 min at 0-5° C. and then added to a solution of 2.15 g of phosphorous pentachloride dissolved in 40 ml of dichloromethane. The reaction mixture was stirred for 30 min at 0-5° C. and 1 h at room temperature. The solvent was evaporated, 100 ml of diethyl ether were added, the mixture was washed once with 150 ml of water, and the organic layer dried over magnesium sulfate, filtered, and the solvent evaporated under reduced pressure. The crude product was purified via silica gel chromatography with n-heptane-dichloromethane (1:1) as eluent to give 0.261 g of the title compound.

1. additionwere added dropwise
2. stirringThe reaction mixture was stirred for 30 min at 0-5° C. and 1 h at room temperature
3. customThe solvent was evaporated
4. addition100 ml of diethyl ether were added
5. washthe mixture was washed once with 150 ml of water
6. dry with materialthe organic layer dried over magnesium sulfate
7. filtrationfiltered
8. customthe solvent evaporated under reduced pressure
9. customThe crude product was purified via silica gel chromatography with n-heptane-dichloromethane (1:1) as eluent

ORDレコード

ord-3b5fd6e5881349f8811421709f2cddf1

出典データセット

uspto-grants-2013_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08470810B2