HRID262763

反应详情

EQUATION

反应方程式

HRID 262763 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 5.85 g. of methyl 3-(2,6-dichlorobenzylidene)thiocarbazimidate hydriodide (U.S. Pat. No. 3,657,337) and 3.24 g. of 2-(aminomethyl)pyridine in 25 ml. of absolute ethanol is heated under reflux for 20 hours and diluted while hot with 75 ml. of water, causing the separation of an oil. On standing, the oil crystallizes and filtration gives 5.00 g. of pale yellow crystals, m.p. 125°-140° C. Recrystallization from aqueous ethanol gives the desired compound as pale yellow crystals, m.p. 159.5°-161° C.

WORKUP

后处理

  1. temperatureunder reflux for 20 hours
  2. additiondiluted while hot with 75 ml
  3. customthe separation of an oil
  4. customthe oil crystallizes
  5. filtrationfiltration
  6. customgives 5.00 g
  7. customRecrystallization from aqueous ethanol