HRID355623

反应详情

EQUATION

反应方程式

HRID 355623 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl-4,4-dimethyl-3-oxovalerate (15.8 g, 0.1 mol) and 2-methoxy-5-nitroaniline (16.8 g, 0.01 mol) were taken up in toluene (150 mL) in a round bottomed flask fitted with a Dean-Stark trap. The mixture was heated to a vigorous reflux while the MeOH side-product was distilled off and removed. After 4 hours, the mixture was cooled and the toluene removed in vacuo. The residue was recrystallized from acetonitrile to yield 27 g of the desired condensation product.

WORKUP

后处理

  1. customfitted with a Dean-Stark trap
  2. temperatureThe mixture was heated to
  3. distillationwas distilled off
  4. customremoved
  5. temperaturethe mixture was cooled
  6. customthe toluene removed in vacuo
  7. customThe residue was recrystallized from acetonitrile
  8. customto yield 27 g of the desired
  9. customcondensation product