HRID1243841

反应详情

EQUATION

反应方程式

HRID 1243841 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3 cm3 of aqueous 1N sodium hydroxide solution are added to a solution of 0.55 g of 3-iodo-6,6-diphenyl-1-(4-toluenesulphonyl)-6,7-dihydro-1H-indazole in 10 cm3 of tetrahydrofuran. After stirring for about 36 hours at a temperature in the region of 20° C., 30 cm3 of ethyl acetate are added. After separation of the phases by settling, the organic phase is washed with three times 15 cm3 of water, 20 cm3 of saturated aqueous sodium chloride solution, dried over magnesium sulphate, filtered and concentrated to dryness under reduced pressure (13 kPa). 0.436 g of 3-iodo-6,6-diphenyl-6,7-dihydro-1H-indazole is obtained in the form of a solid, the characteristics 30′ of which are as follows:

WORKUP

后处理

  1. additionare added
  2. customAfter separation of the phases
  3. washthe organic phase is washed with three times 15 cm3 of water, 20 cm3 of saturated aqueous sodium chloride solution
  4. dry with materialdried over magnesium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated to dryness under reduced pressure (13 kPa)