تفاعل #710480

معادلة التفاعل

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

المردود 26.0%

المذيبات

water

DMF

DMF

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONadded
2. 2
   أخرىwas returned to room temperature
3. 3
   أخرىliquid separation
4. 4
   غسيلThe organic layer was washed with 1% hydrochloric acid
5. 5
   تجفيفdried over anhydrous magnesium sulfate
6. 6
   تركيزconcentrated under reduced pressure
7. 7
   workup.ADDITIONA small amount of hexane and diethyl ether were added
8. 8
   أخرىto precipitate crystals
9. 9
   أخرىthus the crystals were collected
10. 10
    أخرىdried
11. 11
    أخرىto obtain the subject material
12. 12
    أخرىAmount obtained 50 mg (yield 26%)

الإجراء التجريبي

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%).

المصدر