反应 #710480

反应方程式

ethyl acetate

5-bromomethyl-2-fluoropyridine

2,2-difluoro-N-[pyridin-2(1H)-ylidene]acetamide

potassium carbonate

→

2,2-difluoro-N-[1-((6-fluoropyridin-3-yl)methyl)pyridin-2(1H)-ylidene]acetamide

收率 26.0%

溶剂

water

DMF

DMF

反应条件

后处理

1. 1
   workup.ADDITIONadded
2. 2
   其他was returned to room temperature
3. 3
   其他liquid separation
4. 4
   洗涤The organic layer was washed with 1% hydrochloric acid
5. 5
   干燥dried over anhydrous magnesium sulfate
6. 6
   浓缩concentrated under reduced pressure
7. 7
   workup.ADDITIONA small amount of hexane and diethyl ether were added
8. 8
   其他to precipitate crystals
9. 9
   其他thus the crystals were collected
10. 10
    其他dried
11. 11
    其他to obtain the subject material
12. 12
    其他Amount obtained 50 mg (yield 26%)

实验过程

128 mg (0.75 mmol) of 5-bromomethyl-2-fluoropyridine was dissolved in 3 ml of anhydrous DMF, 116 mg (0.68 mmol) of 2,2-difluoro-N-[pyridin-2(1H)-ylidene]acetamide was dissolved in 3 ml of anhydrous DMF and added thereto, and subsequently, 103 mg (0.75 mmol) of potassium carbonate was added thereto and the resulting mixture was stirred at 65° C. for 2 hours. After the reaction was completed, the reaction solution was returned to room temperature, and ethyl acetate and water were added thereto to perform liquid separation. The organic layer was washed with 1% hydrochloric acid, then dried over anhydrous magnesium sulfate and concentrated under reduced pressure. A small amount of hexane and diethyl ether were added thereto to precipitate crystals, and thus the crystals were collected and dried to obtain the subject material. Amount obtained 50 mg (yield 26%).

来源