HRID2294797

反应详情

EQUATION

反应方程式

HRID 2294797 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a similar manner to Example 8, 580 mg (3.30 mmol) of 1-phenyl-imidazolidin-2,4-dione were reacted with560 mg (3.29 mmol) of 3-methoxybenzoyl chloride. After completion of the reaction, pyridine was distilled off under reduced pressure, and the resultant residue was subjected to extraction with ethyl acetate. The organic layer was washed with dilute hydrochloric acid and with saturated saline. The thus-washed organic layer was dried over anhydrous magnesium sulfate, and the solvent was then distilled off. The resultant residue was purified by column chromatography on silica gel (developing solvent: n-hexane/ethyl acetate) and subjected to crystallization from n-hexane/ethyl acetate to obtain 90 mg (yield: 10.2%) of the title compound.

WORKUP

后处理

  1. distillationwas distilled off under reduced pressure
  2. extractionthe resultant residue was subjected to extraction with ethyl acetate
  3. washThe organic layer was washed with dilute hydrochloric acid and with saturated saline
  4. dry with materialThe thus-washed organic layer was dried over anhydrous magnesium sulfate
  5. distillationthe solvent was then distilled off
  6. customThe resultant residue was purified by column chromatography on silica gel (developing solvent: n-hexane/ethyl acetate)
  7. customsubjected to crystallization from n-hexane/ethyl acetate