HRID454505

反应详情

EQUATION

反应方程式

HRID 454505 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Under ice-cooling, concentrated sulfuric acid (1 mL) was added to a methanol (10 mL) suspension of the obtained 2-amino-5-methoxy-4-phenylbenzoic acid, followed by heating to reflux for 6 hours. The reaction mixture was cooled to room temperature and adjusted to a pH of 8.0 with a saturated aqueous solution of sodium bicarbonate, and then chloroform was added thereto. The organic layer was separated and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. Hexane was added to the obtained residue, and the solid substance was collected by filtration to obtain 0.24 g of methyl 2-amino-5-methoxy-4-phenylbenzoate as a brown solid.

WORKUP

后处理

  1. temperatureUnder ice-cooling
  2. temperatureby heating
  3. temperatureto reflux for 6 hours
  4. customThe organic layer was separated
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customthe solvent was evaporated under reduced pressure
  7. additionHexane was added to the obtained residue
  8. filtrationthe solid substance was collected by filtration