反应详情

To a stirred refluxing solution of 5.00 g of 4,6-dichloro-2-methylthiopyrimidine in 150 ml of o-dichlorobenzene under nitrogen was added dropwise 15.00 g of methyl diphenylphosphinite over 35 minutes. The mixture was refluxed for 5.5 hours after the addition was completed and then allowed to cool, at which time it was added to 850 ml of n-hexane. The resulting solid was separated by filtration, washed with n-hexane, and recrystallized from 100 ml of ethanol to give 11.00 g of 4,6-bis(diphenylphosphinyl)-2-methylthiopyrimidine (shown by formula in Claim 8) as white crystals, mp 221°-222° C. Anal. Calcd for C29H24N2O2P2S: C, 66.15; H, 4.59; N, 5.32. Found: C, 65.59; 65.59; H, 4.54, 4.75; N, 5.04, 5.01.

1. temperatureThe mixture was refluxed for 5.5 hours
2. additionafter the addition
3. temperatureto cool, at which time it
4. customThe resulting solid was separated by filtration
5. washwashed with n-hexane
6. customrecrystallized from 100 ml of ethanol