HRID2288160

反应详情

EQUATION

反应方程式

HRID 2288160 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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 3 M 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

  1. temperatureOn cooling
  2. customthe product was partitioned between Et2O and 3 M HCl
  3. extractionThe organic extract
  4. washwas washed with water and brine
  5. dry with materialthen dried (MgSO4)
  6. filtrationfiltered
  7. customevaporated