HRID1955719
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe methanol was evaporated
- extractionThe aqueous phase was extracted with EtOAc
- washThe organic phase was washed with water
- dry with materialdried (MgSO4)
- customevaporated
- customto produce a crude glass which
- customwas recrystallized from EtOAc-hexane