HRID1886314

反应详情

EQUATION

反应方程式

HRID 1886314 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

80 ml of 12N hydrochloric acid was added to 2.0 g of 4-[3-{3-(3-phosphonopropyl)ureido}phenyl]-3-methyl-5-mercaptotriazole (9) thus obtained. The system was allowed to undergo reaction at a temperature of 90° C. over 8 hours. After the completion of the reaction, hydrochloric acid was distilled off under reduced pressure. 20 ml of water was added to the system. The system was then dissolved under heating. Sodium chloride was gradually added to the solution to deposit crystals. The addition of sodium chloride continued until the solution was somewhat whitened. The solution thus whitened was then heated so that it was homogenized. The solution was naturally filtered, and then allowed to stand. As a result, a crystalline 4-[3-{3-(3-phosphonopropyl)ureido}phenyl]-3-methyl-5-mercaptotriazole (10) was deposited. (Yield: 0.58 g (33%); m.p. 195° C.)

WORKUP

后处理

  1. customthus obtained
  2. customreaction at a temperature of 90° C. over 8 hours
  3. distillationwas distilled off under reduced pressure
  4. addition20 ml of water was added to the system
  5. dissolutionThe system was then dissolved
  6. temperatureunder heating
  7. additionSodium chloride was gradually added to the solution to deposit crystals
  8. additionThe addition of sodium chloride
  9. temperatureThe solution thus whitened was then heated so that it
  10. filtrationThe solution was naturally filtered