HRID1153731

反应详情

EQUATION

反应方程式

HRID 1153731 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Approximately 2 g. of 5,8-quinoxalinedione were dissolved in 200 ml. of 2B ethanol. Aniline (1.2 g.) was added and the reaction was stirred overnight at room temperature. The reaction was evaporated, water was added, and the mixture was extracted several times with methylene chloride. The combined extracts were dried over sodium sulfate and evaporated to dryness. The residue was chromatographed over a silica gel column, eluting with ethyl acetate. The desired fractions were combined and evaporated. The material was crystallized from ethyl acetate to give 50 mg. of the title product as a red powder, m.p. about 203°-205° C.

WORKUP

后处理

  1. customThe reaction was evaporated
  2. additionwater was added
  3. extractionthe mixture was extracted several times with methylene chloride
  4. dry with materialThe combined extracts were dried over sodium sulfate
  5. customevaporated to dryness
  6. customThe residue was chromatographed over a silica gel column
  7. washeluting with ethyl acetate
  8. customevaporated
  9. customThe material was crystallized from ethyl acetate
  10. customto give 50 mg