반응 #4960

반응 방정식

benzylmethylamine

oxalic acid

7-chloro-2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]-oxazepine-5(4H)-one

benzylmethylamine

→

white crystals

수율 47.9%

7-Chloro-2,3-dihydro-4-methyl-2-[2-methyl(phenylmethyl)amino]pyrido[3,2-f][1,4]oxazepin-5(4H)-one oxalate

수율 47.9%

용매

isopropyl alcohol

ethanol

반응 조건

후처리

1. 1
   온도the mixture heated
2. 2
   온도to reflux for three days
3. 3
   기타The solvent was removed by rotary evaporation
4. 4
   세척which was subsequently washed with 2×50 ml of dilute sodium hydroxide and 50 ml water
5. 5
   건조dried over sodium sulfate
6. 6
   여과filtered
7. 7
   농축concentrated by rotary evaporation
8. 8
   기타Residual benzylmethylamine was removed at 95° C.
9. 9
   온도the mixture heated
10. 10
    온도to reflux for 24 hrs
11. 11
    기타The resulting crystals were recrystallized from ethanol/isopropyl alcohol

실험 절차

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.

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