HRID1908826
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 60 °C
PROCEDURE
实验过程
A solution of 2-ethyl-6-methyl-isonicotinic acid ethyl ester (3.90 g, 20.2 mmol, prepared in analogy to the corresponding tert.-butyl ester) in 7 N NH3 in methanol (50 mL) is stirred in a sealed vessel at 60° C. for 20 h. The solvent is evaporated and the residue is suspended in diethyl ether. The solid material is collected, washed with additional diethyl ether and dried under HV to give 2-ethyl-6-methyl-isonicotinamide (2.85 g) as a white powder; LC-MS: tR=0.26 min, [M+1]+=165.05; 1H NMR (D6-DMSO): δ 1.23 (t, J=7.5 Hz, 3H), 2.49 (s, 3H), 2.75 (q, J=7.8 Hz, 2H), 7.44 (s, 2H), 7.59 (s br, 1H), 8.11 (s br, 1H).
WORKUP
后处理
- customThe solvent is evaporated
- customThe solid material is collected
- washwashed with additional diethyl ether
- customdried under HV