反应详情

To a suspension of 2.15 (0.085 mole) of sodium hydride in 200 ml dimethylformamide is added 29.1 g (0.075 mole) of 3-{2-nitro-4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]phenyl}-N,N-dimethylpropanamide in in 50 ml dimethylformamide at such a rate that excessive foaming is avoided. To the resulting suspension, stirred in a nitrogen atmosphere, is added 14.2 g (0.10 mole) of methyl iodide to give a reaction mixture, which is stirred at room temperature overnight. The reaction mixture is then treated with 5 ml of ethanol, poured into 1-liter of water and extracted with ether. The resulting ether solution is washed with water, dried over anhydrous magnesium sulfate, filtered and evaporated at reduced pressure to obtain a residual oil which is chromatographed on Silicar® CC-7. Elution with chloroform gives a major fraction consisting of 16 g which is recrystallized from hexane to give 3-{2-nitro-4-[2,2,2-trifluoro-1-methoxy-1-(trifluoromethyl)ethyl]phenyl}-N,N-dimethylpropanamide having a melting point of 51° -54°.

1. customto give a reaction mixture, which
2. stirringis stirred at room temperature overnight
3. extractionextracted with ether
4. washThe resulting ether solution is washed with water
5. dry with materialdried over anhydrous magnesium sulfate
6. filtrationfiltered
7. customevaporated at reduced pressure
8. customto obtain a residual oil which
9. customis chromatographed on Silicar® CC-7
10. washElution with chloroform
11. customgives a major fraction
12. customis recrystallized from hexane