反応 #2383795

反応方程式

sodium iodide

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

potassium carbonate

1-bromopropane

DMF

→

N-(4-Propyl-2,3,4,5-tetrahydro-1,4-benzoxazepin-7-yl)-2-thiophenecarboximidamide hemifumarate

反応条件

後処理

1. 1
   ろ過was then filtered
2. 2
   workup.DISSOLUTIONThe solids were dissolved in water (50 ml)
3. 3
   抽出extracted with methylene chloride (3×50 ml)
4. 4
   乾燥The combined extracts were dried with magnesium sulfate
5. 5
   ろ過filtered
6. 6
   濃縮concentrated to a solid
7. 7
   その他The solids were recrystallized from hot isopropanol
8. 8
   workup.DISSOLUTIONThe solids were dissolved in ethyl acetate
9. 9
   workup.ADDITIONtreated with isopropanol-fumaric acid
10. 10
    その他triturated with ether
11. 11
    ろ過The hemifumarate salt was collected by filtration (0.86 g, 39%), m.p. 174° C.

実験手順

To N-(2,3,4,5-tetrahydro-1,4-benzoxazepin-7-yl)-2-thiophenecarboximidamide (1.57 g, 6 mmol) in DMF (75 ml) was added potassium carbonate (9 g) and 1-bromopropane (1.48 g, 12 mmol) and a catalytic amount of sodium iodide. The mixture was stirred for 48 h and was then filtered. The solids were dissolved in water (50 ml) and extracted with methylene chloride (3×50 ml). The combined extracts were dried with magnesium sulfate, filtered and concentrated to a solid. The solids were recrystallized from hot isopropanol. The solids were dissolved in ethyl acetate, treated with isopropanol-fumaric acid, and triturated with ether. The hemifumarate salt was collected by filtration (0.86 g, 39%), m.p. 174° C.

出典