反应详情

温度

-78 °C

A solution of 0.745 g (0.00150 mol) of 1,1,2-tribromo-2-(2-benzenesulfonyloxyethyl)-cyclopropane in 4 ml of diethyl ether was placed under a nitrogen atmosphere by use of a Firestone valve. While cooling to −78° C. in a dry ice/acetone bath, 23.45 ml (0.00450 mol) of 1.4 M methyl lithium in diethyl ether was added slowly via syringe. After 15 minutes warmed to 0° C. in an ice water bath then returned to −78° C. for about 30 minutes before 2 ml of water was added via syringe. The resulting mixture was transferred to a separatory funnel and the phases were separated. The organic layer was dried over MgSO4 and filtered. The solvent was removed from the filtrate in vacuo with a bath temperature under 20° C. to yield >0.155 g of 70% pure 2-(2-benzenesulfonyloxyethyl)-cyclopropene contaminated with 30% 1-(2-hydroxethyl)cyclopropene as an oil.

1. temperatureAfter 15 minutes warmed to 0° C. in an ice water bath
2. additionwas added via syringe
3. customThe resulting mixture was transferred to a separatory funnel
4. customthe phases were separated
5. dry with materialThe organic layer was dried over MgSO4
6. filtrationfiltered
7. customThe solvent was removed from the filtrate in vacuo with a bath temperature under 20° C.