HRID1262525

反应详情

EQUATION

反应方程式

HRID 1262525 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-(1,3-diethyl-2,3,6,7-tetrahydro-2,6dioxo-1H-purin-8-yl)benzenesulfonic acid (5.0 g, 0.014 moles) and N,N-dimethylformamide (150 ml) is cooled to 0° and treated with thionyl chloride (3.3 g, 0.027 moles). When the addition is complete, the reaction mixture is permitted to warm to ambient temperature and stirred vigorously until a thick slurry results. To this slurry is added N,N-dimethylformamide saturated with ammonia (100 ml). The resulting mixture is then saturated with gaseous ammonia and concentrated on a rotary evaporator. The residue is taken up in water, filtered, triturated with ethanol and dried at 68° C. to yield 2.9 grams of 4-(1,3-diethyl-2,3,6,7-tetrahydro-2,6-dioxo-1H-purin-8-yl)benzenesulfonamide, mp 350°-353° C.(d).

WORKUP

后处理

  1. temperatureis cooled to 0°
  2. additionWhen the addition
  3. customresults
  4. concentrationsaturated with gaseous ammonia and concentrated on a rotary evaporator
  5. filtrationfiltered
  6. customtriturated with ethanol
  7. customdried at 68° C.