反应详情

温度

50 °C

Formic acid (1.0 ml, 26.6 mmol) was added dropwise to 2.0 ml (21.4 mmol) of acetic anhydride in an ice bath. After that, the ice bath was removed, and the solution was stirred at 50° C. for 15 minutes. After allowing to stand for 15 minutes, the resulting solution was cooled again with an ice bath and was added dropwise to a solution of 586 mg (3.55 mmol) of (±)-3-amino-3-phenylpropanoic acid in 0.5 ml of formic acid previously cooled to a temperature not higher than 10° C. The mixture was stirred for 40 minutes as it was, and, when the solution became room temperature, it was stirred for 80 minutes more. The residue prepared by concentrating the reaction solution in vacuo was recrystallized from water to give 624 mg (3.23 mmol) of (±)-3-formylamino-3-phenylpropanoic acid in a yield of 91.0% (melting point: 127 to 128° C.).

1. customAfter that, the ice bath was removed
2. waitto stand for 15 minutes
3. temperaturethe resulting solution was cooled again with an ice bath
4. temperaturepreviously cooled to a temperature not higher than 10° C
5. stirringThe mixture was stirred for 40 minutes as it
6. custombecame room temperature
7. stirringit was stirred for 80 minutes more
8. customThe residue prepared
9. concentrationby concentrating the reaction solution in vacuo
10. customwas recrystallized from water