HRID2185898

反应详情

EQUATION

反应方程式

HRID 2185898 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 3,4-dimethoxy-1-naphthalenecarboxylic acid (2.34 g, 10.1 mmol) and 10% Pd/C (0.56 g) in HOAc (50 mL) was hydrogenated on Parr apparatus at 60° C. and 50 psi for 14 h. After filtration through diatomaceous earth, the solvent was removed in vacuo and water was added. The solid was collected by filtration and washed with water to yield the title compound as a yellow solid (2.21 g, 93%). 1H NMR (DMSO-d6) δ 12.69 (s, 1H), 7.30 (s, 1H), 3.79 (s, 3H), 3.73 (s, 3H), 2.91 (s, 2H), 2.65 (s, 2H), 1.64 (m, 4H); MS m/z 235 (M−H).

WORKUP

后处理

  1. customwas hydrogenated on Parr apparatus at 60° C.
  2. filtrationAfter filtration through diatomaceous earth
  3. customthe solvent was removed in vacuo and water
  4. additionwas added
  5. filtrationThe solid was collected by filtration
  6. washwashed with water