HRID1715239
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of sodium-p-aminosalicylate (Aldrich)(100 g, 0.65 mol) in 10% aqueous NaOH solution (1000 ml) is added 50% wt solution of benzylchloroformate (670 g, 1.96 mol in toluene) at 0° C. The resulting mixture is stirred at rt for 48 h. The progression of the reaction is followed by NMR. The reaction mixture is cooled down to 0° C. and acidified with 10% aqueous HCl. The solid obtained is filtered and washed with cold water and dried. It is further treated with petroleum ether and filtered to give crude 4-{[(benzyloxy)carbonyl]amino}-2-hydroxy benzoic acid (128 g, 68%).
WORKUP
后处理
- temperatureThe reaction mixture is cooled down to 0° C.
- customThe solid obtained
- filtrationis filtered
- washwashed with cold water
- customdried
- additionIt is further treated with petroleum ether
- filtrationfiltered