HRID413696

反应详情

EQUATION

反应方程式

HRID 413696 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-(5-phenyl-benzofuran-2-ylmethoxycarbonylamino)-isonicotinic acid ethyl ester (0.150 g, 0.36 mmol) in THF (3 ml) was added at room temperature 1.0M LiOH (0.72 mL, 0.72 mmol) and the mixture was stirred for 3 h. The solvent was evaporated, water was added, followed by 2N HCl to adjust the pH to 1-2, and the product was extracted with EtOAc. The extract was washed with water, then brine, and dried over magnesium sulfate and concentrated to dryness. Purification by crystallization gave 0.072 g of 3-(5-phenyl-benzofuran-2-ylmethoxycarbonylamino)-isonicotinic acid as a white solid, mp 235.7-238.9° C.

WORKUP

后处理

  1. customThe solvent was evaporated
  2. additionwater was added
  3. extractionthe product was extracted with EtOAc
  4. washThe extract was washed with water
  5. dry with materialbrine, and dried over magnesium sulfate
  6. concentrationconcentrated to dryness
  7. customPurification
  8. customby crystallization