反应详情

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.

1. customThe reaction flask was sealed tightly
2. temperatureafter cooling to 0° C.
3. customto evaporate at room temperature
4. washwashed with dilute aqueous sodium hydroxide (1×30 ml)
5. dry with materialThe chloroform layer was dried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated by rotary evaporation
8. dissolutionThe residual oil was dissolved in hot cyclohexane
9. temperatureUpon cooling
10. custom1.76 g (39.4%) of light yellow crystals were collected