反应详情

温度

135 °C

2-Chloro-N-(2-chloro-4-methyl-3-pyridinyl)-3-pyridine carboxamide (10 g), potassium fluoride (6.17 g), cyclopropylamine (8.08 g) were suspended in o-xylene (30 ml) and heated to 130-140° C. in autoclave for 5-6 h. Then the reaction mass was cooled to 25-30° C., diluted with o-xylene (50 ml) and further heated the reaction mass to 70-75° C. Thereafter, DM water (30 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 (30 ml) at 70-75° C. and organic layer was concentrated at 60-63° C. under reduced pressure. 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 (10 ml, 5-10° C.). Dried the obtained solid at 45-50° 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 (30 ml) at 70-75° C.
5. concentrationorganic layer was concentrated at 60-63° C. under reduced pressure
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 (10 ml, 5-10° C.)
13. customDried the obtained solid at 45-50° C. under reduced pressure