HRID1654303

反应详情

EQUATION

反应方程式

HRID 1654303 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(Procedure B) A stirred mixture of the product from Example 7, Step II, (0.37 g, 0.00128 mol), the product from Step III above (0.298 g, 0.0141 mol), sodium bicarbonate (0.21 g, 0.0026 mol) and acetonitrile (11 ml) was refluxed for 5 hours and kept at ambient temperature for 18 hours. It was filtered and the solid was washed with acetonitrile. The filtrate was concentrated and the residue was chromatographed on silica gel with 10% MeOH--CH2Cl2 to give 0.332 g of the titled product, a compound of Formula I'. The mass spectrum had m/z 416 (M+).

WORKUP

后处理

  1. filtrationIt was filtered
  2. washthe solid was washed with acetonitrile
  3. concentrationThe filtrate was concentrated
  4. customthe residue was chromatographed on silica gel with 10% MeOH