反応 #2383801

反応方程式

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

3-thiophenecarboximidothioic acid, methyl ester, hydroiodide

ammonium hydroxide

→

solid

収率 22.1%

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

収率 22.1%

溶媒

ethanol

water

反応条件

後処理

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

実験手順

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.

出典