反应详情

温度

135 °C

2-Chloro-N-(2-chloro-4-methyl-3-pyridinyl)-3-pyridine carboxamide (100 g), potassium fluoride (22.62 g), cyclopropylamine (80.85 g) were suspended in o-xylene (300 ml) and heated to 130-140° C. in autoclave for 5-9 h. Then the reaction mass was cooled to 25-30° C., diluted with o-xylene (500 ml) and further heated the reaction mass to 70-75° C. Thereafter, DM water (300 ml) added and stirred for 10 min at 70-75° C. The aqueous layer was separated at hot condition and organic layer was washed with DM water (300 ml) at 70-75° C. and organic layer was concentrated at 60-63° C. under reduced pressure up to residue weight attained is approximately 400 g. The concentrated mass was cooled to 25-30° C. and stirred for 15 min and further cooled to 5-10° C. and stirred for 30 min. Filtered the solid obtained and washed with chilled o-xylene (100 ml, 5-10° C.). Dried the obtained solid at 50-60° C. under reduced pressure.

1. temperatureThen the reaction mass was cooled to 25-30° C.
2. temperaturefurther heated the reaction mass to 70-75° C
3. customThe aqueous layer was separated at hot condition and organic layer
4. washwas washed with DM water (300 ml) at 70-75° C.
5. concentrationorganic layer was concentrated at 60-63° C. under reduced pressure up to residue weight
6. temperatureThe concentrated mass was cooled to 25-30° C.
7. stirringstirred for 15 min
8. temperaturefurther cooled to 5-10° C.
9. stirringstirred for 30 min
10. filtrationFiltered the solid
11. customobtained
12. washwashed with chilled o-xylene (100 ml, 5-10° C.)
13. customDried the obtained solid at 50-60° C. under reduced pressure