HRID241744

反应详情

EQUATION

反应方程式

HRID 241744 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Powdered Zn (157.3 mmoles) is added to a solution of the compound obtained in Step F (15.73 mmoles) in glacial acetic acid (150 ml). The reaction mixture is stirred for 6 hours and then filtered. The filtrate is evaporated to dryness and then taken up in water (200 ml) and DCM (400 ml). The phases are separated and the aqueous phase is extracted with DCM; the organic phases are combined. The organic phase obtained is washed with water and then with saturated NaCl solution, dried over sodium sulphate, filtered and evaporated to dryness. The residue obtained is recrystallised from ethanol to yield the title product.

WORKUP

后处理

  1. filtrationfiltered
  2. customThe filtrate is evaporated to dryness
  3. customThe phases are separated
  4. extractionthe aqueous phase is extracted with DCM
  5. customThe organic phase obtained
  6. washis washed with water
  7. dry with materialwith saturated NaCl solution, dried over sodium sulphate
  8. filtrationfiltered
  9. customevaporated to dryness
  10. customThe residue obtained
  11. customis recrystallised from ethanol