反应详情

To a stirred, refluxing mixture of 5.00 g 4,6-dichloropyrimidine in 100 of o-dichlorobenzene under nitrogen was added dropwise 17.00 g of methyl diphenylphosphinite. After the addition was completed, the mixture was refluxed for 6.5 hours and then allowed to cool. The cooled mixture was added to 750 ml of n-hexane, and the white solid that formed was separated by filtration, washed with n-hexane, recrystallized from 150 ml of toluene, and dried at 100° C./0.1 mm (13 Pa) to give 13.64 g of 4,6-bis(diphenylphosphinyl)pyrimidine (shown by formula in Claim 9) as cream-colored crystals, mp 213°-215° C. Anal. Calcd for C28H22N2O2P2 : C, 70.00; H, 4.62; N, 5.83; P, 12.89. Found: C, 69.80; H, 4.65; N, 5.65; P, 12.89.

1. temperatureTo a stirred, refluxing
2. additionAfter the addition
3. temperaturethe mixture was refluxed for 6.5 hours
4. temperatureto cool
5. customthe white solid that formed
6. customwas separated by filtration
7. washwashed with n-hexane
8. customrecrystallized from 150 ml of toluene
9. customdried at 100° C./0.1 mm (13 Pa)