HRID1436663
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
Mix 5-hydroxymethyl-N-methyl-N-propyl-isophthalamic acid ethyl ester (1.0 g, 3.6 mmol), 1 N NaOH (25 mL) in THF (5 mL). Stir at room temperature overnight. Wash with diethyl ether (2×20 mL). Acidify the aqueous layer with 5 N HCl to about pH=2. Extract with ethyl acetate (2×20 mL), concentrate and purify (silica gel chromatography eluting with 1% acetic acid in ethyl acetate and hexanes) to give the title compound (0.80 g, 89%).
WORKUP
后处理
- washWash with diethyl ether (2×20 mL)
- extractionExtract with ethyl acetate (2×20 mL)
- concentrationconcentrate
- custompurify
- wash(silica gel chromatography eluting with 1% acetic acid in ethyl acetate and hexanes)