HRID268638

反应详情

EQUATION

反应方程式

HRID 268638 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

To a solution of 1-(4-fluoro-phenyl)-5-formyl-4-isopropyl-1H-pyrazole-3-carboxylic acid benzylamide (0.620 g, 1.70 mmol) in THF:MeOH (40 mL) at 0° C. was added sodium borohydride (96.3 mg, 2.55 mmol; commercially available from Sigma Aldrich). The reaction was stirred for 30 min at 0° C. at which point TLC analysis indicated the reaction was complete and the solvent was removed under reduced pressure. To the reaction residue was added ethyl acetate (50 mL) and saturated NaHCO3 (15 mL), and the organic layer was separated, dried (Na2SO4) and concentrated. The resulting oil was purified by silica gel chromatography (40% EtOAc/Hex) to afford 1-(4-fluoro-phenyl)-5-hydroxymethyl-4-isopropyl-1H-pyrazole-3-carboxylic acid benzylamide (0.540 g, 87%): MS(APCI+): m/z368.1 (M+H).

WORKUP

后处理

  1. customthe solvent was removed under reduced pressure
  2. additionTo the reaction residue was added ethyl acetate (50 mL) and saturated NaHCO3 (15 mL)
  3. customthe organic layer was separated
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated
  6. customThe resulting oil was purified by silica gel chromatography (40% EtOAc/Hex)