HRID2047276

反应详情

EQUATION

反应方程式

HRID 2047276 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2-dimethylamino-6-vinyl-isonicotinic acid tert-butyl ester (877 mg), 3.53 mmol) in methanol (15 mL), Pd/C (150 mg, 10% Pd) is added and the mixture is stirred under 2 atm of H2 at rt for 3 h. The catalyst is filtered off and the filtrate is evaporated to give crude 2-dimethylamino-6-ethyl-isonicotinic acid tert-butyl ester; LC-MS: tR=0.76 min, [M+1]+=251.10. This material is dissolved in 6 N aq. HCl (60 mL) and the mixture is stirred at 80° C. for 72 h before the solvent is evaporated. The crude product is purified by MPLC on RP-C18-silica gel to give 2-dimethylamino-6-ethyl-isonicotinic acid (332 mg) as an orange oil, LC-MS: tR=0.51 min, [M+1]+=195.10.

WORKUP

后处理

  1. filtrationThe catalyst is filtered off
  2. customthe filtrate is evaporated