反応 #1884993

反応方程式

4-fluoro-benzaldehyde

malonic acid

piperidine

pyridine

HCl

→

4-fluoro-cinnamic acid

収率 90.0%

反応条件

後処理

1. 1
   温度After heating it to 80° C.
2. 2
   workup.STIRRINGthe mixture was stirred for 12 hours
3. 3
   その他After the reaction
4. 4
   温度the resulting solution cooled down to room temperature
5. 5
   ろ過The resulting powder was filtered
6. 6
   洗浄washed with water
7. 7
   その他dried in a vacuum oven

実験手順

10 g (80.6 mmol) of 4-fluoro-benzaldehyde, 29.5 g (2 eq.) of malonic acid, and 1.21 g (0.1 eq.) of piperidine were added to 33.7 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: 90%)

出典