Reaktion #4936

Reaktionsgleichung

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

morpholine

→

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

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe solution was heated
2. 2
   SonstigeThe morpholine was then removed by rotary evaporation (90° C., vacuum pump)
3. 3
   Waschenwashed with dilute aqueous sodium hydroxide (2×30 ml)
4. 4
   EinengenThe organic layer was concentrated by rotary evaporation (60° C., water aspirator)
5. 5
   SonstigeThe residue was recrystallized from ethanol giving 3.26 g (60%) of light yellow crystals, m.p. 152°-153° C.

Vorschrift

2-(2-Chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]oxazepine-5(4H)-thione, 4.5 g (0.018 mole) was dissolved in morpholine (30 ml). The solution was heated with stirring to 50°-60° C. for 6 hr. The morpholine was then removed by rotary evaporation (90° C., vacuum pump). The residue was taken up in chloroform (100 ml) and washed with dilute aqueous sodium hydroxide (2×30 ml). The organic layer was concentrated by rotary evaporation (60° C., water aspirator). The residue was recrystallized from ethanol giving 3.26 g (60%) of light yellow crystals, m.p. 152°-153° C.

Quelle