HRID1842964

反应详情

EQUATION

反应方程式

HRID 1842964 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of dimethyl 2-(2-fluoro-4-nitrophenyl)-2-methylmalonate (1.0 g, 3.50 mmol, 1.0 eq) in methanol (20 mL) was added NaBH4 (0.67 gm, 17.63 mmol, 5.0 eq) at 0° C. and stirred at RT for 16 h. The mixture was diluted with water (20 mL), extracted with ethyl acetate (20 mL). The organic layer was washed with brine, dried over anhydrous Na2SO4, and the solvent was vaporated under reduced pressure. The crude product obtained was purified by CC using EtOAc/PE (2:3) to get 2-(2-fluoro-4-nitrophenyl)-2-methylpropane-1,3-diol (400 mg, 50%; TLC system: EtOAc/PE (1:1), Rf: 0.3).

WORKUP

后处理

  1. extractionextracted with ethyl acetate (20 mL)
  2. washThe organic layer was washed with brine
  3. dry with materialdried over anhydrous Na2SO4
  4. customThe crude product obtained
  5. customwas purified by CC