Reaktion #4934

Reaktionsgleichung

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

2-methyl pyrrolidine

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clear oil

Ausbeute 36.7%

2,3-Dihydro-4-methyl-2-[2-(2-methyl-1-pyrrolidinyl)ethyl]pyrido[3,2-f][1,4]oxazepin-5(4H)-one

Ausbeute 36.7%

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe solution was heated
2. 2
   Temperaturto reflux for 3 hours
3. 3
   SonstigeThe ethanol was removed by rotary evaporation (water aspirator, 80° C.)
4. 4
   SonstigeThe residual oil was partitioned between dilute aqueous sodium hydroxide (50 ml) and chloroform (50 ml)
5. 5
   Extraktionthe aqueous layer extracted with chloroform (2×30 ml)
6. 6
   Trocknendried over anhydrous sodium sulfate
7. 7
   Einengenconcentrated by rotary evaporation (water aspirator, 70° C.)
8. 8
   workup.DISTILLATIONThe residual oil was then distilled at 200° C.

Vorschrift

To a solution of 3.5 g (0.0145 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]oxazepine-5(4H)-one in ethanol (15 ml) was added 2-methyl pyrrolidine (5.0 g, 0.063 mole). The solution was heated to reflux for 3 hours with stirring. The ethanol was removed by rotary evaporation (water aspirator, 80° C.). The residual oil was partitioned between dilute aqueous sodium hydroxide (50 ml) and chloroform (50 ml). The organic layer was saved and the aqueous layer extracted with chloroform (2×30 ml). All the chloroform layers were combined, dried over anhydrous sodium sulfate and concentrated by rotary evaporation (water aspirator, 70° C.). The residual oil was then distilled at 200° C. and low vacuum (vacuum pump) giving 1.5 g (36.7%) of a clear oil.

Quelle