反应详情

温度

50 °C

A solution of Ethyl [S-phenyl-N-(trimethylsilypsulfonimidoyl]acetate (18.7 mmol, obtained as crude oil from step 2) in MeOH—H2O (10:1, 7.5 mL) was treated with cesium fluoride (0.25 g, 1.65 mmol) in one portion. The reaction mixture was heated to 50° C. and stirred for 2 hours. The reaction mixture was concentrated, the residue absorbed to silica gel and purified by chromatography (silica gel, EtOAc-Hexane, Et3N 0.1%). The product containing fractions were concentrated to give the title compound as a pale yellow oil (1.65 g, 39% for steps 1-3).

1. concentrationThe reaction mixture was concentrated
2. customthe residue absorbed to silica gel
3. custompurified by chromatography (silica gel, EtOAc-Hexane, Et3N 0.1%)
4. additionThe product containing fractions
5. concentrationwere concentrated