HRID220452

反应详情

EQUATION

反应方程式

HRID 220452 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

Dissolve 1-methyl-3-trifluoromethyl-1H-pyrazole-4-carboxylic acid ethyl ester (1.74 g, 7.83 mmol) in tetrahydrofuran (100 mL) and cool to 0° C. Add diisobutylaluminum hydride (47.0 mL, 47.0 mmol, 1 M in toluene) dropwise over 15 min. Allow the reaction mixture to warm to room temperature over 16 hr. Partition between ethyl acetate (100 mL) and saturated aqueous potassium sodium tartrate solution (50 mL) and stir at room temperature for another 16 hr. Separate the organic layer; dry (sodium sulfate), filter and concentrate to give (1-methyl-3-trifluoromethyl-1H-pyrazol-4-yl)-methanol (1.42 g, 100%). 1H-NMR (400 MHz, CDCl3) δ 7.42 (s, 1H), 4.63 (s, 2H), 3.90 (s, 3H), 1.80 (bs, 1H).

WORKUP

后处理

  1. temperatureto warm to room temperature over 16 hr
  2. customPartition between ethyl acetate (100 mL) and saturated aqueous potassium sodium tartrate solution (50 mL)
  3. customSeparate the organic layer
  4. dry with materialdry (sodium sulfate)
  5. filtrationfilter
  6. concentrationconcentrate