HRID1363389

反应详情

EQUATION

反应方程式

HRID 1363389 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionpoured onto ice (100 g)
  2. extractionextracted with EtOAc (3×150 mL)
  3. extractionThe organic extract
  4. washwas washed with water
  5. dry with materialdried (anhydrous Na2SO4)
  6. concentrationconcentrated
  7. customThe crude obtained
  8. customwas purified