反応 #433180

反応方程式

diethanolamine

NaOH

diethanolamine

NaOH

2-chloro-4-morpholino-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine

2-Chloro-4-morpholino-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine

product

2-Chloro-4-morpholino-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine

→

2-[Bis-(2-hydroxyethyl)-amino]-4-morpholino-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine

溶媒

water

water

xylene

反応条件

後処理

1. 1
   温度under reflux
2. 2
   workup.STIRRINGafter which the mixture is stirred
3. 3
   温度under reflux for a further 28 hours
4. 4
   温度to cool
5. 5
   洗浄washed with water
6. 6
   その他the organic phase is separated off
7. 7
   乾燥After drying over Na2SO4
8. 8
   その他evaporating
9. 9
   その他recrystallizing twice from toluene
10. 10
    その他the above product is obtained as a white powder which melts at 135°-140°

実験手順

5.3 g of diethanolamine and a solution of 1 g of NaOH in 3 ml of water are added to a solution of 20 g of 2-chloro-4-morpholino-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine (product from Example 44) in 50 ml of xylene. 1 g of NaOH in 3 ml of water is again added after 1.75 hours with stirring under reflux. After 14 hours, 7.9 g of diethanolamine are added, after which the mixture is stirred under reflux for a further 28 hours. It is then allowed to cool and washed with water, and the organic phase is separated off. After drying over Na2SO4, evaporating and recrystallizing twice from toluene, the above product is obtained as a white powder which melts at 135°-140°.

出典