HRID1047847

反应详情

EQUATION

反应方程式

HRID 1047847 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The solution of 2-bromo-3-methyl-benzoic acid (1.5 g, 6.98 mmol) in 10 mL THF is treated with 1M Bu2Mg/heptane at −15° C. under argon. After stirring for 30 min, 1.6M n-BuLi/hexane is added dropwise at −15° C. and the mixture is left for 1 hr. Then isobutyryl chloride (2.95 ml, 27.9 mmol) is added dropwise. After another 30 min stirring, the reaction is quenched with 2N HCl aqueous solution (2 ml). After concentration, the residue is purified by HPLC to give a pure product (227) as white solid (840 mg, 58%).

WORKUP

后处理

  1. waitthe mixture is left for 1 hr
  2. stirringAfter another 30 min stirring
  3. customthe reaction is quenched with 2N HCl aqueous solution (2 ml)
  4. concentrationAfter concentration
  5. customthe residue is purified by HPLC