تفاعل #1884995

معادلة التفاعل

3,4-di-fluoro-benzaldehyde

malonic acid

piperidine

pyridine

HCl

→

3,4-di-fluoro-cinnamic acid

المردود 95.0%

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter heating it to 80° C.
2. 2
   workup.STIRRINGthe mixture was stirred for 12 hours
3. 3
   أخرىAfter the reaction
4. 4
   درجة الحرارةthe resulting solution cooled down to room temperature
5. 5
   ترشيحThe resulting powder was filtered
6. 6
   غسيلwashed with water
7. 7
   أخرىdried in a vacuum oven

الإجراء التجريبي

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%)

المصدر