反应详情

To a stirred, refluxing mixture of 3.56 g of 5-bromo-4-chloro-2-methylthiopyrimidine in 100 ml of o-dichlorobenzene under nitrogen was added dropwise 10.00 g of methyl diphenylphosphinite. After the addition was completed, the mixture was refluxed for 6 hours and then allowed to cool. Volatiles were removed from the mixture under vacuum, and the residue was recrystallized from 30 ml of 1-chlorobutane and dried at 50° C./0.1 mm (13 Pa) to give 2.97 g of 5-bromo-4-diphenylphosphinyl-2-methylthiopyrimidine (shown by formula in Claim 7) as white crystals, mp 124°-127° C. Anal. Calcd for C17H14BrN2OPS: C, 50.39; H, 3.48; N, 6.91. Found: C, 50.54; H, 3.67; N, 6.84.

1. temperatureTo a stirred, refluxing
2. additionAfter the addition
3. temperaturethe mixture was refluxed for 6 hours
4. temperatureto cool
5. customVolatiles were removed from the mixture under vacuum
6. customthe residue was recrystallized from 30 ml of 1-chlorobutane
7. customdried at 50° C./0.1 mm (13 Pa)