反应详情

0.400 g (1.49 mmol) of the above prepared [6-(4-trifluoromethoxy-phenyl)-pyridin-3-yl]-methanol was dissolved in 7.2 ml of CH2Cl2 and treated dropwise at 0° C. with 0.22 ml (2 eq.) of SOCl2. The reaction mixture was kept at 0° C. for 5 Min. and at RT for 30 Min. Pouring onto crashed ice/NaHCO3, twofold extraction with AcOEt, washing with water, drying over sodium sulfate, and evaporation of the solvents produced 0.419 g of pure title compound as off-white solid of mp. 34–36° C.

1. customwas kept at 0° C. for 5 Min
2. customat RT
3. additionPouring
4. extractionice/NaHCO3, twofold extraction with AcOEt
5. washwashing with water
6. dry with materialdrying over sodium sulfate, and evaporation of the solvents