HRID1293441

反应详情

EQUATION

反应方程式

HRID 1293441 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Intermediate 38 (550 mg, 2.26 mmol) was taken in methanol (10 ml) and raney nickel catalyst (100 mg, 18% w/w) was added. The reaction mixture was refluxed and to this was added hydrazine hydrate (99%) solution (2 ml) slowly over a period of 10 min. The refluxing continued for 2 h. The catalyst was filtered and the filterate was concentrated and diluted with water (100 ml) and further extracted with ethyl acetate (3×25 ml). The organic layer was washed with water and concentrated to give the product as brown solid (500 mg);mp: 167-169° C.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed
  2. filtrationThe catalyst was filtered
  3. concentrationthe filterate was concentrated
  4. additiondiluted with water (100 ml)
  5. extractionfurther extracted with ethyl acetate (3×25 ml)
  6. washThe organic layer was washed with water
  7. concentrationconcentrated