反应 #2328987

反应方程式

6-Chloro-N-(2-hydroxy-4-methoxyphenyl)nicotinamide

methylamine

→

title compound

N-(2-Hydroxy-4-methoxyphenyl)-6-(methylamino)nicotinamide

溶剂

methanol

反应条件

后处理

1. 1
   其他The solvent was evaporated in vacuo
2. 2
   其他the residue was partitioned between water and ethyl acetate
3. 3
   萃取The aqueous layer was extracted five
4. 4
   干燥organics were dried (MgSO4)
5. 5
   过滤filtered
6. 6
   其他evaporated
7. 7
   过滤filtered
8. 8
   其他dried

实验过程

6-Chloro-N-(2-hydroxy-4-methoxyphenyl)nicotinamide (0.40 g, 1.44 mol) was mixed with a solution of 8M methylamine in methanol (4 mL) and heated in a microwave reactor at 250° C. for 10 minutes. The solvent was evaporated in vacuo and the residue was partitioned between water and ethyl acetate. The aqueous layer was extracted five timed with ethyl acetate The pooled organics were dried (MgSO4), filtered and evaporated. The solid was titurated with CH2Cl2, filtered and dried, giving the title compound (0.25 g) as a solid. 1H NMR δ ppm 9.73 (s, 1H) 9.38 (s, 1H) 8.65 (d, 1H) 7.92 (dd, 1H) 7.33 (d, 1H) 7.16 (d, 1H) 6.24-6.58 (m, 3H) 3.70 (s, 3H) 2.83 (d, 3H); MS m/z (M+H) 274; (M−H) 272.

来源