HRID442125

反应详情

EQUATION

反应方程式

HRID 442125 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

4-Amino-6,7-dimethoxy-2-(7-nitro-1,2,3,4-tetrahydroisoquinolin-2-yl)quinazoline (2.0 g.), the product of Example 12. was slurried in 6N hydrochloric acid solution (100 ml.) and the resulting mixture was cooled with stirring to 0° C. A solution of stannous chloride (20.0 g) in 6N hydrochloric acid (20 ml.) was then added, and the reaction mixture was heated gradually to 70° C., followed by cooling to give a white solid precipitate. The latter material was collected by means of suction filtration and thereafter recrystallized from ethanol to afford 1.0 g. of pure final product as the dihydrochloride dihydrate, m.p. 265°-266° C.

WORKUP

后处理

  1. temperaturethe resulting mixture was cooled
  2. temperaturethe reaction mixture was heated gradually to 70° C.
  3. temperatureby cooling
  4. customto give a white solid precipitate
  5. filtrationThe latter material was collected by means of suction filtration
  6. customrecrystallized from ethanol
  7. customto afford 1.0 g