Reaktion #4937

Reaktionsgleichung

2-(2-Chloroethyl)-4-ethyl-2,3-dihydropyrido[3,2-f][1,4]oxazepin-5(4H)-thione hydrochloride

dimethylamine

dimethylamine

→

2-[2-(Dimethylamino)ethyl]-4-ethyl-2,3-dihydropyrido [3,2-f][1,4]oxazepin-5(4H)-thione

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe reaction flask was sealed tightly
2. 2
   Temperaturafter cooling to 0° C.
3. 3
   Sonstigeto evaporate at room temperature
4. 4
   Waschenwashed with dilute aqueous sodium hydroxide (1×30 ml)
5. 5
   TrocknenThe chloroform layer was dried over sodium sulfate
6. 6
   Filtrationfiltered
7. 7
   Einengenconcentrated by rotary evaporation
8. 8
   workup.DISSOLUTIONThe residual oil was dissolved in hot cyclohexane
9. 9
   TemperaturUpon cooling
10. 10
    Sonstige1.76 g (39.4%) of light yellow crystals were collected

Vorschrift

2-(2-Chloroethyl)-4-ethyl-2,3-dihydropyrido[3,2-f][1,4]oxazepin-5(4H)-thione hydrochloride, 5.00 g (0.016 mole) was added to 20 ml of anhydrous dimethylamine. The reaction flask was sealed tightly and stirred at room temperature for 6 days. The flask was opened after cooling to 0° C. and dimethylamine allowed to evaporate at room temperature. The residue was taken up in chloroform (100 ml) and washed with dilute aqueous sodium hydroxide (1×30 ml). The chloroform layer was dried over sodium sulfate, filtered and concentrated by rotary evaporation. The residual oil was dissolved in hot cyclohexane. Upon cooling, 1.76 g (39.4%) of light yellow crystals were collected, m.p. 73° C.

Quelle