反应详情

To a suspension of 1-(3-fluorophenyl)-2-(5-trifluoromethyl-2-pyridinyl)ethanone oxime (10.0 g, 33.53 mmol) in DME (38 ml) was added MsCl (2.6 ml, 33.53 mmol) at 0° C. The suspension was stirred for 15-20 min and then Et3N (9.3 ml, 67.1 mmol) dissolved in DME (4 ml) was added dropwise at a rate to maintain the temperature ≦5° C. After the addition was complete, the suspension was warmed to room temperature and stirred for 1 hour. Additional Et3N (0.47 ml, 3.35 mmol) was added and the solution was stirred for 15 min at 30-35° C. The suspension was cooled to room temperature and filtered to remove the salts. The cake was washed with twice with DME (10 ml) and the filtrate was transferred to a clean reaction flask. To the filtrate was added FeCl2 (42 mg, 0.34 mmol) at room temperature. The solution was heated to 70° C. and stirred for 30 min. After cooling the solution to 40° C., H2O was added (80 ml). The resultant suspension was cooled to 0-5° C. and stirred for 30 min. The solid was isolated by filtration and partially dried via airflow. The solid was further dried under reduced pressure (20 in Hg Vacuum) at 50° C. to afford 7.91 g (84%) of the title compound as a beige solid.

1. additionwas added dropwise at a rate
2. temperatureto maintain the temperature ≦5° C
3. additionAfter the addition
4. stirringstirred for 1 hour
5. stirringthe solution was stirred for 15 min at 30-35° C
6. temperatureThe suspension was cooled to room temperature
7. filtrationfiltered
8. customto remove the salts
9. washThe cake was washed with twice with DME (10 ml)
10. customthe filtrate was transferred to a clean reaction flask
11. temperatureThe solution was heated to 70° C.
12. stirringstirred for 30 min
13. temperatureAfter cooling the solution to 40° C.
14. stirringstirred for 30 min
15. customThe solid was isolated by filtration
16. custompartially dried via airflow
17. customThe solid was further dried under reduced pressure (20 in Hg Vacuum) at 50° C.