HRID978075

反应详情

EQUATION

反应方程式

HRID 978075 的结构方程式

PROCEDURE

实验过程

Concentrated sulfuric acid (40 ml) was carefully added to a solution of 2,6-dihydroxybenzoic acid (133 g, 0.86 mol) in absolute methanol (500 ml). The reaction mixture was heated at reflux temperature for 24 hours, cooled, and evaporated. The residue was added to aa saturated sodium hydrogencarbonate solution, and the resulting solid was collected by filtration, washed with water, and dried in vacuo over phosphorus peroxide; yield 49 g (34%). NMR (CDCl3, 60 MHz): δ4.02 (s, CO2CH3) p.p.m.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux temperature for 24 hours
  3. temperaturecooled
  4. customevaporated
  5. additionThe residue was added to aa saturated sodium hydrogencarbonate solution
  6. filtrationthe resulting solid was collected by filtration
  7. washwashed with water
  8. dry with materialdried in vacuo over phosphorus peroxide