반응 #1884995

반응 방정식

3,4-di-fluoro-benzaldehyde

malonic acid

piperidine

pyridine

HCl

→

3,4-di-fluoro-cinnamic acid

수율 95.0%

반응 조건

후처리

1. 1
   온도After heating it to 80° C.
2. 2
   workup.STIRRINGthe mixture was stirred for 12 hours
3. 3
   기타After the reaction
4. 4
   온도the resulting solution cooled down to room temperature
5. 5
   여과The resulting powder was filtered
6. 6
   세척washed with water
7. 7
   기타dried in a vacuum oven

실험 절차

10 g (70.4 mmol) of 3,4-di-fluoro-benzaldehyde, 14.65 g (2 eq.) of malonic acid, and 0.59 g (0.1 eq.) of piperidine were added to 16.7 g (3 eq.) of pyridine and stirred at room temperature for about 1 hour. After heating it to 80° C., the mixture was stirred for 12 hours. After the reaction, the resulting solution cooled down to room temperature and was slowly added with 1M HCl until it was titrated to about pH 4. The resulting powder was filtered and washed with water, and then dried in a vacuum oven. (Yield: 95%)

출처