HRID909105

反应详情

EQUATION

反应方程式

HRID 909105 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 4-cyano-2-methoxy-benzoic acid methyl ester (1.01 g, 5.28 mmol) in methanol (50 mL) was added to Raney-nickel 2800 slurry in water (a few grams washed with methanol to remove the water, Aldrich) and it was put under a 50 psi hydrogen atmosphere for 16 hrs. The mixture was filtered through Celite under an argon atmosphere and concentrated and then purified by flash chromatography to give 4-aminomethyl-2-methoxy-benzoic acid methyl ester (385.7 mg, 34.7%).

WORKUP

后处理

  1. washwashed with methanol
  2. customto remove the water, Aldrich) and it
  3. filtrationThe mixture was filtered through Celite under an argon atmosphere
  4. concentrationconcentrated
  5. custompurified by flash chromatography