HRID862347
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
1-Bromo-2-hydroxy-4-methoxybenzene. 3-Bromo-2-hydroxy-6-methoxybenzoic acid [T. de Paulis et. al., J. Med. Chem., (1985), 28, 1263-1269] (5 g, 0.02 mol) was heated in quinoline (200 mL) at 160° C. for 1 h. On cooling, the product was partitioned between Et2O and 3M HCl. The organic extract was washed with water and brine then dried (MgSO4), filtered and evaporated to give the title compound which was recrystallized from 5% ethyl acetate/hexane (4 g, 97%); m.p. 40°-42° C. Anal. Calc. for C7H7BrO2 : C, 41.41; H, 3.48. Found C, 41.39; H, 3.37.
WORKUP
后处理
- temperatureOn cooling
- customthe product was partitioned between Et2O and 3M HCl
- extractionThe organic extract
- washwas washed with water and brine
- dry with materialthen dried (MgSO4)
- filtrationfiltered
- customevaporated