HRID253696

反应详情

EQUATION

反应方程式

HRID 253696 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a solution of methyl-6-chloro-3-(4-ethylphenylamino)benzo[d]isoxazole-7-carboxylate (211 mg, 638 μmol) in dioxane (10.5 ml) was added a 1N aqueous solution of LiOH hydrate (134 mg, 3190 μmol) and the resulting mixture was heated to 50° C. After 1 hr, the solvent was removed in vacuo, the residue was diluted with H2O and acidified to pH2 with 2N HCl. After diluting with EtOAc, the layers were separated and the aqueous layer was extracted with EtOAc (3×). The organics were combined, washed with brine, dried over MgSO4, filtered and concentrated to obtain the title compound as a brown solid, which was used without further purification.

WORKUP

后处理

  1. customthe solvent was removed in vacuo
  2. additionthe residue was diluted with H2O
  3. additionAfter diluting with EtOAc
  4. customthe layers were separated
  5. extractionthe aqueous layer was extracted with EtOAc (3×)
  6. washwashed with brine
  7. dry with materialdried over MgSO4
  8. filtrationfiltered
  9. concentrationconcentrated