HRID1530847

反应详情

EQUATION

反应方程式

HRID 1530847 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of the product from Example 16 (0.53 g, 1.32 mmol) in 3N HCl (50 mL) was treated with oxalic acid (0.25 g, 1.98 mmol) and refluxed for four hours. After cooling to room temperature, the precipitate was filtered, suspended in water (70 mL), heated to 80° C. and basifyed to pH 8. The solids were filtered, and dried to give the title compound in two crops [125 mg, mp=293-297° C. (dec.)] and [33 mg, mp=263-266° C. (dec.)] yielding 34%.

WORKUP

后处理

  1. temperaturerefluxed for four hours
  2. filtrationthe precipitate was filtered
  3. temperatureheated to 80° C. and basifyed to pH 8
  4. filtrationThe solids were filtered
  5. customdried