反応 #1375006

反応方程式

ether

1,8-Diaminonaphthalene

2-hydroxy-2-methyl butyric acid

hydrochloric acid

ethanol

→

α-ethyl-α-methyl-2-perimidinemethanol, hydrochloride

反応条件

後処理

1. 1
   温度heated
2. 2
   温度under reflux for 96 hours
3. 3
   温度to cool
4. 4
   ろ過is filtered
5. 5
   その他yielding a gray-green solid
6. 6
   温度The solid is heated
7. 7
   ろ過is filtered while hot
8. 8
   その他to remove unreacted
9. 9
   濃縮The filtrate is concentrated to dryness
10. 10
    workup.ADDITIONthe resulting solid is treated with 500 ml of boiling ethanol
11. 11
    その他After the insoluble material is removed by filtration
12. 12
    workup.ADDITIONthe filtrate was treated with charcoal
13. 13
    その他yielding a yellow solution
14. 14
    温度cooling
15. 15
    その他yields a yellow-brown solid
16. 16
    その他Recrystallization from ethanol (charcoal)

実験手順

1,8-Diaminonaphthalene (44.5 g, 0.282 mole) is suspended in 400 ml of 4N hydrochloric acid. To this suspension is added 2-hydroxy-2-methyl butyric acid (50 g, 0.423 mole) and the whole is stirred and heated under reflux for 96 hours. Then the reaction mixture is allowed to cool and is filtered, yielding a gray-green solid. The solid is heated and stirred with 1 liter of refluxing ethanol, and is filtered while hot to remove unreacted starting materials. The filtrate is concentrated to dryness and the resulting solid is treated with 500 ml of boiling ethanol. After the insoluble material is removed by filtration, the filtrate was treated with charcoal, yielding a yellow solution. Addition of ether, plus cooling, yields a yellow-brown solid. Recrystallization from ethanol (charcoal) yields the desired product, α-ethyl-α-methyl-2-perimidinemethanol, hydrochloride, m.p. 266°-268° dec.).

出典