HRID1186954

反应详情

EQUATION

反应方程式

HRID 1186954 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

In a 250 ml round bottom flask, 3-bromo-2-methoxybenzoic acid (4.0 g, 17 mmol, 1.0 eq) was dissolved in THF (100 mL). The solution was cooled to 0° C. To above solution was added dropwise borane/THF complex (1 N, 17.3 mL, 17.3 mmol). The solution was warmed to r.t. and let stirred at r.t for 15 hr. The reaction was quenched with addition of aqueous ammonium chloride and concentrated. The mixture was diluted with EtOAc, washed with 1 N HCl followed by aqueous sodium bicarbonate solution, brine and water. The organic phase was dried over MgSO4, filtered and concentrated. The crude product was used without purification.

WORKUP

后处理

  1. additionTo above solution was added dropwise borane/THF complex (1 N, 17.3 mL, 17.3 mmol)
  2. temperatureThe solution was warmed to r.t.
  3. customThe reaction was quenched with addition of aqueous ammonium chloride
  4. concentrationconcentrated
  5. additionThe mixture was diluted with EtOAc
  6. washwashed with 1 N HCl
  7. dry with materialThe organic phase was dried over MgSO4
  8. filtrationfiltered
  9. concentrationconcentrated
  10. customThe crude product was used without purification