Реакция #2383801

Уравнение реакции

2,3,4,5-Tetrahydro-1,4-benzoxazepin-7-ylamine hydrochloride

3-thiophenecarboximidothioic acid, methyl ester, hydroiodide

ammonium hydroxide

→

solid

Выход 22.1%

N-(2,3,4,5-Tetrahydro-1,4-benzoxazepin-7-yl)-3-thiophenecarboximidamide

Выход 22.1%

Растворители

ethanol

water

Условия реакции

Обработка

1. 1
   Температураheated at 60° C. overnight
2. 2
   Температураcooled
3. 3
   ДругоеThe solid (1.02 g) was collected
4. 4
   ДругоеThe filtrate was evaporated
5. 5
   workup.ADDITIONthe residue treated with ethyl acetate
6. 6
   ДругоеThe resulting crystals were collected
7. 7
   Другоеobtained previously
8. 8
   Экстракцияextracted with methylene chloride (3×30 ml)
9. 9
   ПромывкаThe organic extracts were washed with water
10. 10
    Сушкаdried over magnesium sulfate
11. 11
    Концентрированиеconcentrated

Методика

2,3,4,5-Tetrahydro-1,4-benzoxazepin-7-ylamine hydrochloride (1.84 g, 8.4 mmol) was dissolved in 95% ethanol (40 ml) and 3-thiophenecarboximidothioic acid, methyl ester, hydroiodide (2.85 g, 10 mmol) was added. The mixture was stirred at room temperature for 2 days and then heated at 60° C. overnight and cooled. The solid (1.02 g) was collected. The filtrate was evaporated and the residue treated with ethyl acetate. The resulting crystals were collected and combined with the solid obtained previously. They were dissolved in water (20 ml), basified with conc. ammonium hydroxide, and extracted with methylene chloride (3×30 ml). The organic extracts were washed with water, dried over magnesium sulfate, and concentrated to give a solid (0.508 g), m.p. 150-152° C.

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