HRID552951

反应详情

EQUATION

反应方程式

HRID 552951 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 5-nitroindole (38) (3.0 g, 18.501 mmol) in dry methanol (50 mL) was treated with KOH (5.6 g) at room temperature. After stirring for 10 min., 1,4-cyclohexanedione monoethylene ketal (7.22 g, 46.253 mmol) was added and the resulting solution was refluxed for 36 h. The reaction was brought to room temperature and solvent was evaporated. Crude was diluted with water (50 mL), precipitated solid was filtered off and washed with water (2 10 mL). The precipitate was dried under vacuum to obtain compound 78 (4.7 g, 85%) as a solid. For spectral data, please see Example 23.

WORKUP

后处理

  1. temperaturethe resulting solution was refluxed for 36 h
  2. customwas brought to room temperature
  3. customsolvent was evaporated
  4. additionCrude was diluted with water (50 mL)
  5. customprecipitated solid
  6. filtrationwas filtered off
  7. washwashed with water (2 10 mL)
  8. customThe precipitate was dried under vacuum