HRID1955719

反应详情

EQUATION

反应方程式

HRID 1955719 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of the product produced in step B (1.25 g, 3.9 mmol), K2 CO3 (3.5 g, 25.3 mmol) and 60 ml MeOH/H2O 1:1 was refluxed for 3 h. The methanol was evaporated, and the aqueous residue acidified to pH 1 using 6N HCl. The aqueous phase was extracted with EtOAc. The organic phase was washed with water, dried (MgSO4), and evaporated to produce a crude glass which was recrystallized from EtOAc-hexane to afford 1.1 g of the title compound as a solid, m. p. 198°-201° C.

WORKUP

后处理

  1. customThe methanol was evaporated
  2. extractionThe aqueous phase was extracted with EtOAc
  3. washThe organic phase was washed with water
  4. dry with materialdried (MgSO4)
  5. customevaporated
  6. customto produce a crude glass which
  7. customwas recrystallized from EtOAc-hexane