تفاعل #4960
ord-c3bc64bc129e484f957dfe469d616691
معادلة التفاعل
المتفاعلات
الكواشف
المذيبات
ظروف التفاعل
المعالجة
- 1درجة الحرارةthe mixture heated
- 2درجة الحرارةto reflux for three days
- 3أخرىThe solvent was removed by rotary evaporation
- 4غسيلwhich was subsequently washed with 2×50 ml of dilute sodium hydroxide and 50 ml water
- 5تجفيفdried over sodium sulfate
- 6ترشيحfiltered
- 7تركيزconcentrated by rotary evaporation
- 8أخرىResidual benzylmethylamine was removed at 95° C.
- 9درجة الحرارةthe mixture heated
- 10درجة الحرارةto reflux for 24 hrs
- 11أخرىThe resulting crystals were recrystallized from ethanol/isopropyl alcohol
الإجراء التجريبي
To a solution of 6.0 g (0.022 mole) of 7-chloro-2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]-oxazepine-5(4H)-one in 50 ml of absolute ethanol was added 5.3 g (0.044 mole) of benzylmethylamine and the mixture heated to reflux for three days. The solvent was removed by rotary evaporation, and the residue was taken up in 100 ml of methylene chloride, which was subsequently washed with 2×50 ml of dilute sodium hydroxide and 50 ml water, dried over sodium sulfate, filtered, and concentrated by rotary evaporation. Residual benzylmethylamine was removed at 95° C., 0.5 mm Hg. However, the mass spectrum now showed starting material; therefore, the residue was taken up in 50 ml of absolute ethanol. To the resulting solution was added 2.7 g (0.022 mole) of benzylmethylamine and the mixture heated to reflux for 24 hrs. The reaction mixture was subjected to the same work-up as mentioned before. The syrup was treated with oxalic acid in isopropyl alcohol. The resulting crystals were recrystallized from ethanol/isopropyl alcohol to give 4.7 g (47.9%) of white crystals, m.p. 176°-179° C.