HRID732519

反应详情

EQUATION

反应方程式

HRID 732519 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. washWash with diethyl ether (2×20 mL)
  2. extractionExtract with ethyl acetate (2×20 mL)
  3. concentrationconcentrate
  4. custompurify
  5. wash(silica gel chromatography eluting with 1% acetic acid in ethyl acetate and hexanes)