反応 #2328987

反応方程式

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

methylamine

→

title compound

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

溶媒

methanol

反応条件

後処理

1. 1
   その他The solvent was evaporated in vacuo
2. 2
   その他the residue was partitioned between water and ethyl acetate
3. 3
   抽出The aqueous layer was extracted five
4. 4
   乾燥organics were dried (MgSO4)
5. 5
   ろ過filtered
6. 6
   その他evaporated
7. 7
   ろ過filtered
8. 8
   その他dried

実験手順

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.

出典