반응 #451602

반응 방정식

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

반응 조건

후처리

1. 1
   기타The reaction flask was sealed tightly
2. 2
   온도after cooling to 0° C.
3. 3
   기타to evaporate at room temperature
4. 4
   세척washed with dilute aqueous sodium hydroxide (1×30 ml)
5. 5
   건조The chloroform layer was dried over sodium sulfate
6. 6
   여과filtered
7. 7
   농축concentrated by rotary evaporation
8. 8
   workup.DISSOLUTIONThe residual oil was dissolved in hot cyclohexane
9. 9
   온도Upon cooling
10. 10
    기타1.76 g (39.4%) of light yellow crystals were collected

실험 절차

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.

출처