反应详情

温度

135 °C

2-Chloro-N-(2-chloro-4-methyl-3-pyridinyl)-3-pyridine carboxamide (15 g), trisodium phosphate dodecahydrate (20.21 g), cyclopropylamine (12.12 g) were suspended in o-xylene (45 ml) and heated to 130-140° C. for 6-8 h in S.S. Bomb with occasional shaking. Then the reaction mass was cooled to 70-75° C., diluted with o-xylene (75 ml) and DM water (45 ml) and stirred for 10 min at 70-80° C. The aqueous layer was separated and washed the organic layer with DM water (45 ml) at 70-80° C. The organic layer was concentrated at 60-65° C. under reduced pressure. The concentrated mass was cooled to 5-10° C. and stirred for 30 min. Filtered the solid obtained and washed with chilled o-xylene (15 ml, 5-10° C.). Dried the obtained solid at 55-60° C. under reduced pressure.

1. temperatureThen the reaction mass was cooled to 70-75° C.
2. customThe aqueous layer was separated
3. washwashed the organic layer with DM water (45 ml) at 70-80° C
4. concentrationThe organic layer was concentrated at 60-65° C. under reduced pressure
5. temperatureThe concentrated mass was cooled to 5-10° C.
6. stirringstirred for 30 min
7. filtrationFiltered the solid
8. customobtained
9. washwashed with chilled o-xylene (15 ml, 5-10° C.)
10. customDried the obtained solid at 55-60° C. under reduced pressure