تفاعل #985278

ord-a527c186e6e543a2ae93c96fe96c45dd

معادلة التفاعل

O=Cc1ccc([N+](=O)[O-])cc1
p-nitro-benzaldehyde
O=C(O)CC(=O)O
malonic acid
CC(=O)O
Acetic acid
CC(=O)[O-].[NH4+]
ammonium acetate
CC(=O)[O-].[NH4+]
ammonium acetate
N[C@H](CC(=O)O)c1ccc([N+](=O)[O-])cc1
p-nitro-β-phenylalanine
المردود 52.0%

المذيبات

ظروف التفاعل

درجة الحرارة
85°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةheated at 90° C.
  2. 2
    درجة الحرارةAfter being cooled to room temperature
  3. 3
    ترشيحThe precipitated crystal was filtered
  4. 4
    غسيلto slurry washing with 100 ml of ethanol
  5. 5
    ترشيحfiltered again
  6. 6
    أخرىdried under reduced pressure

الإجراء التجريبي

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%.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07351571B2uspto-grants-2008_04