反应 #985278

ord-a527c186e6e543a2ae93c96fe96c45dd

反应条件

温度
85°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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%.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07351571B2uspto-grants-2008_04