تفاعل #2557
ord-237b1973c5eb44b6bba25ecc54bfc269
معادلة التفاعل
المتفاعلات
الكواشف
ظروف التفاعل
المعالجة
- 1أخرىat room temperature
- 2أخرىthe solvent was removed by evaporation
- 3workup.DISTILLATIONthe resulting residue was subjected to azeotropic distillation
- 4أخرىto obtain an orange glutinous material
- 5أخرىat room temperature
- 6workup.STIRRINGAfter 2 hours of stirring at the same temperature
- 7استخلاصextracted with ethyl acetate
- 8غسيلwashed with water and saturated brine
- 9تجفيفThe resulting organic layer was dried on anhydrous sodium carbonate
- 10أخرىthe solvent was removed by evaporation
- 11أخرىthe resulting residue was purified
الإجراء التجريبي
1-(2,2-Diethoxyethyl)-4-(4-fluorobenzoyl)piperidine (81 mg, 0.25 mmol) was dissolved in THF (3 ml) to which was subsequently added 10% hydrochloric acid (2 ml) at room temperature. After 1 hour of stirring at the same temperature, the solvent was removed by evaporation, and the resulting residue was subjected to azeotropic distillation using benzene (5 ml×4) to obtain an orange glutinous material. The thus obtained residue was dissolved in methanol (2 ml) to which were subsequently added o-anisidine (29 μl, 0.25 mmol) and sodium cyanoborohydride (11 mg, 0.166 mmol) at room temperature. After 2 hours of stirring at the same temperature, the reaction solution was mixed with saturated sodium carbonate aqueous solution (10 ml), extracted with ethyl acetate and then washed with water and saturated brine. The resulting organic layer was dried on anhydrous sodium carbonate, the solvent was removed by evaporation and then the resulting residue was purified by subjecting it to a silica gel column chromatography (ether:hexane=2:1-ether) to obtain 59 mg (66.2%) of the title compound in the form of colorless solid.