HRID1363389
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
CONDITIONS
反应条件
- 温度
- 25 °C
PROCEDURE
实验过程
Compound of example 127 (2 g, 4.14 mmol) was stirred with H3PO4 (6N, 50 mL) at 100° C. for 1.5 h. The solution was cooled to 25° C. and poured onto ice (100 g). It was made basic using a saturated aqueous Na2CO3 solution and extracted with EtOAc (3×150 mL). The organic extract was washed with water, dried (anhydrous Na2SO4), and concentrated. The crude obtained was purified using a silica gel column and 10% methanol+1% liquor NH3 in CHCl3 as eluant to furnish the title compound.
WORKUP
后处理
- additionpoured onto ice (100 g)
- extractionextracted with EtOAc (3×150 mL)
- extractionThe organic extract
- washwas washed with water
- dry with materialdried (anhydrous Na2SO4)
- concentrationconcentrated
- customThe crude obtained
- customwas purified