تفاعل #2328987

معادلة التفاعل

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

methylamine

→

title compound

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

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   أخرىThe solvent was evaporated in vacuo
2. 2
   أخرىthe residue was partitioned between water and ethyl acetate
3. 3
   استخلاصThe aqueous layer was extracted five
4. 4
   تجفيفorganics were dried (MgSO4)
5. 5
   ترشيحfiltered
6. 6
   أخرىevaporated
7. 7
   ترشيحfiltered
8. 8
   أخرىdried

الإجراء التجريبي

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.

المصدر