HRID77506

反应详情

EQUATION

反应方程式

HRID 77506 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To NaOH (1 M in water; 18.7 mL; 18.7 mmol) is added S-methylisothiourea sulphate (4.25 g; 15.3 mmol). The mixture is stirred until complete dissolution is achieved. CH2Cl2: tetrahydrofuran (1:1; 30 mL) and then 1-(tert-butylcarbamoyl)prop-1-en-2-yl 3,5-diamino-6-chloropyrazine-2-carboxylate (Intermediate 2; 2.00 g; 6.10 mmol) are added and the mixture is stirred at room temperature over night. The organic solvents are evaporated, then water (50 mL) is added. The precipitate formed is collected by filtration while applying suction, washed successively with water, methanol and then with diethyl ether and then dried at 50° C. to yield the title compound (1.33 g, 84% of theory).

WORKUP

后处理

  1. stirringthe mixture is stirred at room temperature over night
  2. customThe organic solvents are evaporated
  3. additionwater (50 mL) is added
  4. customThe precipitate formed
  5. filtrationis collected by filtration
  6. washwashed successively with water, methanol
  7. dry with materialwith diethyl ether and then dried at 50° C.