HRID985403

反应详情

EQUATION

反应方程式

HRID 985403 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-chloro-6-methoxy-pyridazine (100 g), thiourea (105 g) and ethyl methyl ketone (1.8 L) was prepared and refluxed for three hours. The reaction mixture was then cooled and the supernatant was poured into water and extracted with 1M sodium hydroxide (4×100 mL). The sodium hydroxide solution was washed with ethyl acetate (2×50 mL) and the aqueous extract was acidified with sufficient concentrated hydrochloric acid to lower the pH to 5. The resulting yellow solid was collected and air dried to afford the title compound (24%, 23 g); mp, 198-200° C.

WORKUP

后处理

  1. customwas prepared
  2. temperaturerefluxed for three hours
  3. temperatureThe reaction mixture was then cooled
  4. extractionextracted with 1M sodium hydroxide (4×100 mL)
  5. washThe sodium hydroxide solution was washed with ethyl acetate (2×50 mL)
  6. extractionthe aqueous extract
  7. customThe resulting yellow solid was collected
  8. customair dried