تفاعل #607461
ord-189b2f97cecc4c6ca9715ea316809a7f
معادلة التفاعل
المتفاعلات
الكواشف
المذيبات
ظروف التفاعل
المعالجة
- 1workup.ADDITIONThe following were added to a 250 mL reactor
- 2أخرىwere removed slowly with the assistance of a Dean-Stark
- 3workup.ADDITIONTo the resulting mixture, 100 mL of an aqueous solution of acetic acid were added at 10% and 150 mL of ethyl acetate
- 4أخرىthe organic phase separated
- 5غسيلwashed with 2 portions of 50 mL of a 5% sodium bicarbonate solution
- 6تجفيفdry with MgSO4
- 7ترشيحfiltered
- 8أخرىevaporated to dryness
- 9أخرىyielding the raw product as a slightly yellowish oil
- 10درجة الحرارةThis agitation was maintained for two hours in order
- 11أخرىthe precipitation of the hydrochloride
- 12ترشيحThe resulting solid was filtered
- 13أخرىvacuum dried
الإجراء التجريبي
The following were added to a 250 mL reactor: 3-(2-chloroethyl) quinazoline-4 (3H)-one (1 g, 4.79 mmol), 1-(3-(trifluoromethyl)phenyl)piperazine (1,103 g, 4.79 mmol), sodium carbonate (0.762 g, 7.19 mmol), sodium iodide (0.072 g, 0.479 mmol), ethanol (50 ml) and toluene (150 ml). The reaction medium was kept under agitation and reflux for a period of twenty hours, during which 150 ml of the solvent were removed slowly with the assistance of a Dean-Stark. To the resulting mixture, 100 mL of an aqueous solution of acetic acid were added at 10% and 150 mL of ethyl acetate. The mixture was agitated, the organic phase separated, washed with 2 portions of 50 mL of a 5% sodium bicarbonate solution, dry with MgSO4, filtered and evaporated to dryness, yielding the raw product as a slightly yellowish oil. This oil was dissolved in isopropanol, adding 2 mL of concentrated HCl under agitation to the resulting solution. This agitation was maintained for two hours in order to complete the precipitation of the hydrochloride. The resulting solid was filtered and vacuum dried, yielding 1.45 g of 3-(2-(4-(3-(trifluoromethyl)phenyl)piperazine-1-yl)ethyl)quinazoline-4 (3H)-one hydrochloride (3.3 mmol, yield=69%).