反应详情

A mixture of 2-methoxy-4-trifluoromethyl benzaldehyde (Description 96; 18 g, 88 mmol) and lithium chloride (11.19 g; 264 mmol) in anhydrous N,N-dimethylformamide (100 ml) was heated at reflux for 3 hours. The mixture was cooled and poured into water (200 ml), then acidified by the addition of 1N HCl. The mixture was extracted with ether (3×200 ml) then the combined ether layers washed with water (2×500 ml), sat NaCl (100 ml), dried over Na2SO4, filtered and evaporated to give the title compound (16.25 g, 97%).

1. temperaturewas heated
2. temperatureat reflux for 3 hours
3. temperatureThe mixture was cooled
4. extractionThe mixture was extracted with ether (3×200 ml)
5. washthe combined ether layers washed with water (2×500 ml)
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. customevaporated