Reacción #2383801

Ecuación de reacción

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

3-thiophenecarboximidothioic acid, methyl ester, hydroiodide

ammonium hydroxide

→

solid

Rendimiento 22.1%

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

Rendimiento 22.1%

Disolventes

ethanol

water

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturaheated at 60° C. overnight
2. 2
   Temperaturacooled
3. 3
   OtroThe solid (1.02 g) was collected
4. 4
   OtroThe filtrate was evaporated
5. 5
   workup.ADDITIONthe residue treated with ethyl acetate
6. 6
   OtroThe resulting crystals were collected
7. 7
   Otroobtained previously
8. 8
   Extracciónextracted with methylene chloride (3×30 ml)
9. 9
   LavadoThe organic extracts were washed with water
10. 10
    Secadodried over magnesium sulfate
11. 11
    Concentraciónconcentrated

Procedimiento

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.

Fuente