HRID1796328
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureAfter cooling it
- extractionThen it was extracted with EtOAc (3×100 mL each)
- customthe combined organic extracts were dried
- washThe residue was washed with ether