反应 #2383801

反应方程式

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

3-thiophenecarboximidothioic acid, methyl ester, hydroiodide

ammonium hydroxide

→

solid

收率 22.1%

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

收率 22.1%

溶剂

ethanol

water

反应条件

后处理

1. 1
   温度heated at 60° C. overnight
2. 2
   温度cooled
3. 3
   其他The solid (1.02 g) was collected
4. 4
   其他The filtrate was evaporated
5. 5
   workup.ADDITIONthe residue treated with ethyl acetate
6. 6
   其他The resulting crystals were collected
7. 7
   其他obtained previously
8. 8
   萃取extracted with methylene chloride (3×30 ml)
9. 9
   洗涤The organic extracts were washed with water
10. 10
    干燥dried over magnesium sulfate
11. 11
    浓缩concentrated

实验过程

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.

来源