HRID1796328

反应详情

EQUATION

反应方程式

HRID 1796328 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

[3-(4-Methoxybenzenesulfonyl)-6-methyl-pyridin-2-yl]-(2,4,6-trimethylphenyl)-amine from Example 9 (3.0 g, 7.57 mmol) was heated in 48% HBr (40 mL) at 110° C. for 48 h. After cooling it was diluted with water (100 mL) and neutralized with Na2CO3. Then it was extracted with EtOAc (3×100 mL each) and the combined organic extracts were dried and stripped in vacuo. The residue was washed with ether to give 4-[6-methyl-2-(2,4,6-trimethylphenylamino)-pyridine-3-sulfonyl]-phenol as a solid (2.6 g), mp 226–228° C. mass spec. (AP+): m/z 383 (M+1).

WORKUP

后处理

  1. temperatureAfter cooling it
  2. extractionThen it was extracted with EtOAc (3×100 mL each)
  3. customthe combined organic extracts were dried
  4. washThe residue was washed with ether