反应详情

To a 250 mL 3-neck RBF equipped with a condenser, magnetic stirrer, thermo-probe, nitrogen purge and pressure-equilibrated addition funnel was added benzoyl isothiocyanate (25.0 g, 0.150 mol) followed by dichloromethane (100 mL). The mixture was cooled in an ice-water bath at a temperature below 5° C., at which point diacetamide (15.3 g, 0.150 mol) and acetone as the solvent and dichloromethane (100 mL) were added slowly over a period of time of about 30 minutes. The ice-water bath was removed and the reaction mixture was stirred under a nitrogen purge overnight. The reaction mixture was then concentrated in vacuo at a temperature of 40° C. and then dried to constant weight in vacuo at a temperature of 50° C. and a pressure of <1 mTorr.

1. customTo a 250 mL 3-neck RBF equipped with a condenser, magnetic stirrer
2. customthermo-probe, nitrogen purge
3. additionwere added slowly over a period of time of about 30 minutes
4. customThe ice-water bath was removed
5. custompurge overnight
6. concentrationThe reaction mixture was then concentrated in vacuo at a temperature of 40° C.
7. customdried to constant weight in vacuo at a temperature of 50° C.