HRID267237

反应详情

EQUATION

反应方程式

HRID 267237 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 5 g. (0.0187 mole) of 7-chloro-1,2-dihydro-4-methyl-5-phenylpyrrolo[3,2,1-hi]indole in 400 ml. of glacial acetic acid was treated with ozone at room temperature until all the suspended material went into solution, the reaction mixture was poured into water and the mixture extracted with chloroform. The chloroform extracts were combined and concentrated to an oil. The oil was treated with a solution of 100 ml. of hydrochloric acid and 100 ml. of glacial acetic acid; the mixture was refluxed four hours and then poured into water. The solution was extracted with chloroform, the solution dried and concentrated to an oil. The oil was dissolved in benzene and chromatographed on 50 g. of magnesium silicate. The material was molecularly distilled to give 1.5 g. (33%) of product. The yellow product melted at 114°-117°C.

WORKUP

后处理

  1. additionA suspension of 5 g
  2. extractionthe mixture extracted with chloroform
  3. concentrationconcentrated to an oil
  4. additionThe oil was treated with a solution of 100 ml
  5. temperaturethe mixture was refluxed four hours
  6. additionpoured into water
  7. extractionThe solution was extracted with chloroform
  8. customthe solution dried
  9. concentrationconcentrated to an oil
  10. dissolutionThe oil was dissolved in benzene
  11. customchromatographed on 50 g
  12. distillationThe material was molecularly distilled
  13. customto give 1.5 g