HRID1242359

反应详情

EQUATION

反应方程式

HRID 1242359 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.582 g (2.062 mmol) of the above prepared 6-(4-trifluoromethyl-phenyl)-pyridazine-3-carboxylic acid methyl ester in 20 ml of abs. THF was cooled down to −15° C. and reacted with 5.16 ml of DIBAL-H-solution (1.0 M in toluene, 2.5 eq.) for ½ h. Careful quenching with ice/HCl dil., twofold extraction with AcOEt, washing with water, drying over sodium sulfate, and evaporation of the solvents left a crude product which was purified by flash chromatography (SiO2, AcOEt) to yield 0.155 g of the title compound as light brown solid.

WORKUP

后处理

  1. customCareful quenching with ice/HCl dil., twofold extraction with AcOEt
  2. washwashing with water
  3. dry with materialdrying over sodium sulfate, and evaporation of the solvents
  4. waitleft a crude product which
  5. customwas purified by flash chromatography (SiO2, AcOEt)