反应详情

温度

0 °C

A solution of DMSO (1.7 eq.) in DCM (0.5 M) was treated at −78° C. with a 2 M solution of oxalyl chloride in DCM (1.4 eq.). The reaction was stirred for 5 min, and a solution of 2-(4-fluorophenyl)-2-methylpropan-1-ol (1 eq.) in DCM (3 M) added to the reaction mixture. After stirring for 10 min, NEt3 (2.4 eq.) was added and the reaction mixture warmed to 0° C., stirred one hour, removed the cooling bath and stirred for one additional hour. The mixture was diluted with DCM, extracted with bleach/water, 1 M citric acid, water, dried (Na2SO4), concentrated.

1. stirringAfter stirring for 10 min
2. stirringstirred one hour
3. customremoved the cooling bath
4. stirringstirred for one additional hour
5. additionThe mixture was diluted with DCM
6. extractionextracted with bleach/water, 1 M citric acid, water
7. dry with materialdried (Na2SO4)
8. concentrationconcentrated