HRID463971

反应详情

EQUATION

反应方程式

HRID 463971 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.0 grams (0.014 mole) of the product of Example 1 was reacted with 2.37 grams (0.014 mole) of 2-nitrobutyl acetate in 100 mls of dry pyridine. This solution was heated to reflux for 1 hour, cooled and the solvent distilled at reduced pressure. The residual solid was recrystallized from methyl alcohol to give 2.0 grams (37% yield) of a white-yellow solid melting at 154°-155° C. The infrared spectrum showed the C-C band at 3.5μ, the nitrile band at 4.5μ, and the amide carbonyl band at 6.0μ.

WORKUP

后处理

  1. temperatureThis solution was heated
  2. temperatureto reflux for 1 hour
  3. temperaturecooled
  4. distillationthe solvent distilled at reduced pressure
  5. customThe residual solid was recrystallized from methyl alcohol