HRID223801

反应详情

EQUATION

反应方程式

HRID 223801 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4,5-Dichloro-6-methoxy-2,3-dihydro-1H-indene (21 gm., 0.097 mole) is dissolved in acetic acid (280 ml.) and chromium trioxide (14 gm., 0.14 mole) in a mixture of water (15 ml.) and acetic acid (40 ml.) is added dropwise with stirring over a period of one hour. The mixture is poured, with stirring into cold water (1200 ml.) and the solid that separates is removed by filtration, washed with water and dried. The product, which consists of a mixture of the desired material and the isomer described in Step D, is subjected to column chromatographic separation using 225 gm. of silica gel and chloroform is used for elution. Evaporation of the solvent gives 6,7-dichloro-5-methoxy-2,3-dihydro-1H-inden-1-one, 5.2 gm., m.p. 154°-156° C.

WORKUP

后处理

  1. additionis added dropwise
  2. additionThe mixture is poured
  3. customthe solid that separates is removed by filtration
  4. washwashed with water
  5. customdried
  6. additionThe product, which consists of a mixture of the desired material
  7. customis subjected to column chromatographic separation
  8. washof silica gel and chloroform is used for elution
  9. customEvaporation of the solvent