تفاعل #953208

معادلة التفاعل

1-[(N-methylsulfonyl-N-methylamino)-sulfonyl]-3-(N-methylsulfonyl-N-methylamino)urea

2-amino-4,6-di-methoxypyrimidine

→

desired product

المردود 103.2%

1- [(N-Methylsulfonyl-N-methyl-amino) -sulfonyl]-3- (4,6-dimethoxy-2-pyrimidyl) urea

المردود 103.2%

المذيبات

chlorobenzene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter cooling to 20° C.
2. 2
   ترشيحthe precipitate is filtered off
3. 3
   غسيلwashed with 100 ml of chlorobenzene

الإجراء التجريبي

32.3 g of 1-[(N-methylsulfonyl-N-methylamino)-sulfonyl]-3-(N-methylsulfonyl-N-methylamino)urea are slurried in 500 ml of chlorobenzene, 15.5 g of 2-amino-4,6-di-methoxypyrimidine are added at 80° C. with stirring, and the mixture is heated for 3 hours at 80° C. After cooling to 20° C., the precipitate is filtered off and washed with 100 ml of chlorobenzene. 36.4 g of the desired product are obtained with a purity of 98.1%, corresponding to a yield of 96.8% of theory. The melting point for the product is 183°-185° C. 5.1 g of N-methylmethanesulfonamide are recovered from the liltrate by distillation, corresponding to a yield of 92.7% of theory.

المصدر