反応 #2383794

反応方程式

water

water

2,3,4,5-tetrahydro-1,4-benzoxazepin-7-ylamine

2-thiophenecarboximidothioic acid, methyl ester, hydroiodide

→

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

溶媒

DMF

反応条件

後処理

1. 1
   ろ過The solids were collected by filtration
2. 2
   workup.DISSOLUTIONThe solid was dissolved in hot ethyl acetate
3. 3
   ろ過filtered
4. 4
   workup.ADDITIONdiluted with hexane
5. 5
   ろ過The solids were collected by filtration (3.13 g, 64%), MS m/Z 274 [M+H]+

実験手順

To 2,3,4,5-tetrahydro-1,4-benzoxazepin-7-ylamine (3.67 g, 18 mmol) in DMF (60 ml) was added 2-thiophenecarboximidothioic acid, methyl ester, hydroiodide (5.52 g, 19 mmol). The mixture was heated to 50° C. for 24 h. The mixture was poured into water (50 ml), then basic water (150 ml) and was allowed to stir for 1 h. The solids were collected by filtration. The solid was dissolved in hot ethyl acetate, filtered, and diluted with hexane. The solids were collected by filtration (3.13 g, 64%), MS m/Z 274 [M+H]+.

出典