反応 #985278

反応方程式

p-nitro-benzaldehyde

malonic acid

Acetic acid

ammonium acetate

ammonium acetate

→

p-nitro-β-phenylalanine

収率 52.0%

溶媒

2-propanol

反応条件

後処理

1. 1
   温度heated at 90° C.
2. 2
   温度After being cooled to room temperature
3. 3
   ろ過The precipitated crystal was filtered
4. 4
   洗浄to slurry washing with 100 ml of ethanol
5. 5
   ろ過filtered again
6. 6
   その他dried under reduced pressure

実験手順

Acetic acid (110 ml) was mixed with 20.4 g of ammonium acetate (264 mmol) and heated to 85° C. After ammonium acetate was dissolved, the mixture was further mixed with 20.0 g of p-nitro-benzaldehyde (132 mmol) and 27.8 g of malonic acid (264 mmol) and heated at 90° C. with stirring for 5 hours. After being cooled to room temperature, the filtrate was mixed with 300 ml of 2-propanol. The precipitated crystal was filtered, subjected to slurry washing with 100 ml of ethanol, filtered again and dried under reduced pressure to give 14.4 g of p-nitro-β-phenylalanine at a yield of 52.0%.

出典