2-CHLORO-N-PYRIDIN-2-YL-ACETAMIDE synthesis
- Product Name:2-CHLORO-N-PYRIDIN-2-YL-ACETAMIDE
- CAS Number:5221-37-4
- Molecular formula:C7H7ClN2O
- Molecular Weight:170.6
Yield:5221-37-4 97%
Reaction Conditions:
Stage #1: 2-aminopyridine;chloroacetyl chloride in 1,2-dichloro-ethane at 80; for 0.0833333 h;Microwave irradiation;
Stage #2: with sodium hydroxide in water;1,2-dichloro-ethane;
Steps:
1.1
2-aminopyridine (2.8 g, 30 mmol) was dissolved in dichloroethane (25 ml) in a 50 ml-glass vessel and chloroacetyl chloride was added dropwise thereto. The glass vessel was capped with a TFM teflon cover and placed in a rotor in a microwave reactor. The mixture was irradiated by microwave at 300 W and 80° C., for 5 min. After irradiating for 5 min., the reaction mixture was adjusted to pH9 with a saturated aqueous solution of sodium hydroxide and extracted twice with dichloroethane. The organic layer was dried over anhydrous sodium sulfate. The solvent was removed by using a rotary evaporator and the desired pink solid product of 4.9 g (97%) was obtained by recrystallization with acetonitrile. mp 110-115° C.; IR (KBr) 3443, 3226, 1683, 1581, 1330, 1198, 775 cm-1; 1H NMR (CDCl3) 4.2 (2H, s), 7.1 (1H, d), 7.7 (1H, t), 8.2 (1H, d, J=8.3 Hz), 8.4 (1H, d, J=4.9 Hz), 8.95 (1H, bs); 13C NMR (CDCl3) 43.2, 111.4, 121.0, 139.1, 148.2, 150.7, 164.9; EIMS m/z 170.6 (M+)
References:
US2007/36715,2007,A1 Location in patent:Page/Page column 4-5
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