反応 #412452

反応方程式

disodium N-acetoacetylaspartate

phosphorous trichloride

L-phenylalanine methyl ester

N-acetoacetyl-L-aspartic anhydride

→

N-acetoacetyl-L-aspartyl-L-phenylalanine methyl ester

溶媒

acetic acid

ethyl acetate

dioxane

反応条件

後処理

1. 1
   workup.ADDITIONwas added dropwise
2. 2
   温度to warm to ambient temperatures
3. 3
   workup.STIRRINGAfter continued stirring for 20 hours
4. 4
   その他the solvent was evaporated under vacuum at 35°-40° C
5. 5
   workup.ADDITIONToluene, 200 parts by volume, was added to the residue
6. 6
   その他the evaporation

実験手順

Crude disodium N-acetoacetylaspartate, 28.51 parts, was stirred with 200 parts by volume of ethyl acetate and 11.7 parts by volume of acetic acid at 0°-5° C. under argon while 4.37 parts by volume of phosphorous trichloride was added dropwise. The resulting mixture was allowed to warm to ambient temperatures while stirring for 20 hours. To the resulting solution which contains N-acetoacetyl-L-aspartic anhydride was added dropwise over a 2 hour period 122 parts by volume of 0.9 M L-phenylalanine methyl ester in dioxane. After continued stirring for 20 hours, the solvent was evaporated under vacuum at 35°-40° C. Toluene, 200 parts by volume, was added to the residue and the evaporation was repeated, giving crude N-acetoacetyl-L-aspartyl-L-phenylalanine methyl ester as a semi-solid yellow residue.

出典