反应详情

温度

0 °C

In a 10 ml Schlenk tube, 3.5 mg of dry zinc chloride was dissolved in 3.0 ml of absolute tetrahydrofuran and cooled to 0° C. under argon. Thereafter, 279 mg of tert-butyl (S)-2-trifluoromethanesulphonyloxypropionate (ee>99%) and 0.700 ml of n-butylmagnesium chloride (2.00 M solution in THF) were added in succession and the reaction was stirred for 3 h at 0° C. Thereafter, the reaction mixture was diluted with petroleum ether, first water and then saturated ammonium chloride solution were added and the organic phase was separated off. This was applied directly to a silica gel filter and washed with petroleum ether. The product was then washed off with a petroleum ether/diethyl ether mixture (10:1) from the filter and freed from the solvent. The pure tert-butyl (S)-2-methylhexanoate (entry 3 in table 1)(ee>99%) was obtained in quantitative yield.

1. customthe organic phase was separated off
2. filtrationfilter
3. washwashed with petroleum ether
4. washThe product was then washed off with a petroleum ether/diethyl ether mixture (10:1) from the
5. filtrationfilter