HRID1633472

反应详情

EQUATION

反应方程式

HRID 1633472 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-{[Cyano-(2,3,5-trichlorophenyl)-methyl]-amino}-acetamidine hydrobromide (95.36 g, 0.256 mole) was added in portions to a solution of lithium hydroxide monohydrate (16.11 g, 0.384 mole) in methanol (1.9 litres) at room temperature. The resulting solution was stirred at room temperature for 3 hours before being evaporated to dryness in vacuo. The resulting solid was slurried in water (1.15 litres) and collected by filtration. After drying at 50° C. in vacuo the crude material was purified by recrystallisation from toluene to give the desired product. Yield 69.51 g (93.8%), M.p. 178-180° C.

WORKUP

后处理

  1. custombefore being evaporated to dryness in vacuo
  2. filtrationcollected by filtration
  3. dry with materialAfter drying at 50° C. in vacuo the crude material
  4. customwas purified by recrystallisation from toluene