HRID989370

反应详情

EQUATION

反应方程式

HRID 989370 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

A solution of 4.7 g (12.0 mmol) of 3-amino-6-benzyloxy-7-methoxynaphthalene-2-carboxylic acid tert-butyl ester and 2.0 g of 10% Pd/C in 40 mL of DMF and 100 mL of methanol is shaken on Parr shaker at 40 psi for 18 hours. The catalyst is filtered through a pad of Celite, washed with methanol and solvent is evaporated to yield a residue which is dissolved in methylene chloride. This is then filtered through a short pad of Magnesol and washed with methylene chloride and ethyl acetate. The filtrate is evaporated to yield 3.4 g of 3-amino-6-hydroxy-7-methoxynaphthalene-2-carboxylic acid tert-butyl ester as a yellow solid, mp 262-263° C.

WORKUP

后处理

  1. filtrationThe catalyst is filtered through a pad of Celite
  2. washwashed with methanol and solvent
  3. customis evaporated
  4. customto yield a residue which
  5. filtrationThis is then filtered through a short pad of Magnesol
  6. washwashed with methylene chloride and ethyl acetate
  7. customThe filtrate is evaporated