Реакция #4937

Уравнение реакции

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

Условия реакции

Обработка

1. 1
   ДругоеThe reaction flask was sealed tightly
2. 2
   Температураafter cooling to 0° C.
3. 3
   Другоеto evaporate at room temperature
4. 4
   Промывкаwashed with dilute aqueous sodium hydroxide (1×30 ml)
5. 5
   СушкаThe chloroform layer was dried over sodium sulfate
6. 6
   Фильтрацияfiltered
7. 7
   Концентрированиеconcentrated by rotary evaporation
8. 8
   workup.DISSOLUTIONThe residual oil was dissolved in hot cyclohexane
9. 9
   ТемператураUpon cooling
10. 10
    Другое1.76 g (39.4%) of light yellow crystals were collected

Методика

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.

Источник