HRID978075
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperatureThe reaction mixture was heated
- temperatureat reflux temperature for 24 hours
- temperaturecooled
- customevaporated
- additionThe residue was added to aa saturated sodium hydrogencarbonate solution
- filtrationthe resulting solid was collected by filtration
- washwashed with water
- dry with materialdried in vacuo over phosphorus peroxide