反应详情

温度

15 °C

To the concentrated hydrochloric acid (250 ml), 25.0 gm of 2-amino-6-methoxy-3-nitropyridine (0.147 mole) was added at room temperature. The resulting solution was cooled to 15° C. and 66.7 gm of stannous chloride dihydrate (0.294 mole) was added slowly. The reaction mass was heated to 35°–40° C. and mixed for 5–6 hrs with constant stirring. The reaction was monitored by TLC. After the reaction was over, the reaction mixture was cooled to 20° C. and stirred for one hour. The resulting mixture was filtered and dried to give 27.0 gm of 2,3-diamino-6-methoxypyridine dihydrochloride (yield=86.4%); Melting point 211 to 213° C.; HPLC purity was 99.0%.

1. temperatureThe reaction mass was heated to 35°–40° C.
2. additionmixed for 5–6 hrs with constant stirring
3. temperaturewas cooled to 20° C.
4. filtrationThe resulting mixture was filtered
5. customdried