反应详情

温度

60 °C

To a solution of 0.12 g (0.265 mmol) N-(3,5-bis-trifluoromethyl-benzyl)-N-methyl-3-o-tolyl-isonicotinamide in 3 ml tetrahydrofuran 1.6 ml of a 1M solution of BH3 in tetrahydrofuran was added and the reaction mixture stirred for 16 h at 60° C. After addition of 2 ml 3M HCl in ether the reaction mixture was stirred for 3 h at 60° C. The solution was cooled to room temperature and 5 ml 3N sodium hydroxide solution and 10 ml ethyl acetate were added. Stirring was continued for ½ h, the phases separated and the aqueous phase extracted twice with 15 ml ethyl acatate. The combined organic layers were washed with brine, dried (magnesium sulfate) and evaporated. Chromatography of the residue afforded 0.30 g (25%) of the title compound as a pale yellow oil.

1. stirringwas stirred for 3 h at 60° C
2. temperatureThe solution was cooled to room temperature
3. stirringStirring
4. waitwas continued for ½ h
5. customthe phases separated
6. extractionthe aqueous phase extracted twice with 15 ml ethyl acatate
7. washThe combined organic layers were washed with brine
8. dry with materialdried (magnesium sulfate)
9. customevaporated