HRID1242359
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customCareful quenching with ice/HCl dil., twofold extraction with AcOEt
- washwashing with water
- dry with materialdrying over sodium sulfate, and evaporation of the solvents
- waitleft a crude product which
- customwas purified by flash chromatography (SiO2, AcOEt)