HRID916660

反应详情

EQUATION

反应方程式

HRID 916660 的结构方程式

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 4-chloro-6-methyl-5-propyl-pyrimidine (101) (500 mg, 2.93 mmol) and hydrazine monohydrate (880 mg, 17.6 mmol) in EtOH (15 mL) is heated in a sealed tube at 100° C. overnight. On cooling, the solvent is removed and to the residue is added water (15 mL). The solid is filtered and washed with water (5 mL) and ether (10 mL). The solid is then heated in acetic acid (10 mL) in a sealed tube at 110° C. overnight. The excess acetic acid is removed under vacuum. The residue is neutralized with aqueous sodium bicarbonate and then extracted with ethyl acetate. On drying, the solvent is removed to give the product (168).

WORKUP

后处理

  1. temperatureOn cooling
  2. customthe solvent is removed and to the residue
  3. additionis added water (15 mL)
  4. filtrationThe solid is filtered
  5. washwashed with water (5 mL) and ether (10 mL)
  6. temperatureThe solid is then heated in acetic acid (10 mL) in a sealed tube at 110° C. overnight
  7. customThe excess acetic acid is removed under vacuum
  8. extractionextracted with ethyl acetate
  9. customOn drying
  10. customthe solvent is removed