HRID22616

反应详情

EQUATION

反应方程式

HRID 22616 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A flask equipped with a stirrer and a thermometer was charged with 26.98 g of the intermediate 3-bromo-7-nitrodibenzothiophene-5-oxide prepared in Example 1-2 and 269.8 g of glacial acetic acid in a nitrogen atmosphere. 112.7 g of SnCl2.2H2O dissolved in 158 g of concentrated hydrochloric acid was added dropwise at 14 to 18° C. over 1 hour, and stirred overnight at room temperature. The resulting reactant was filtered, washed with 1:1 glacial acetic acid/concentrated hydrochloric acid, and neutralized with 1100 g of a 7 wt % aqueous solution of sodium hydroxide. The reactant was extracted with ethyl acetate, washed with water, concentrated, and purified by silica gel chromatography using 1:1 hexane/chloroform mixed with 0.1 wt % triethylamine as an eluting solvent, to thereby obtain 17.31 g of objective 7-bromodibenzothiophene-3-yl-amine. The product was subjected to elemental analysis, the results of which are as follows:

WORKUP

后处理

  1. customA flask equipped with a stirrer
  2. additionwas added dropwise at 14 to 18° C. over 1 hour
  3. filtrationThe resulting reactant was filtered
  4. washwashed with 1:1 glacial acetic acid/concentrated hydrochloric acid
  5. extractionThe reactant was extracted with ethyl acetate
  6. washwashed with water
  7. concentrationconcentrated
  8. custompurified by silica gel chromatography
  9. additionmixed with 0.1 wt % triethylamine as an eluting solvent