反応 #2148

反応方程式

sodium hydride

3-phenylxanthine

benzyl bromide

→

7-Benzyl-3-phenylxanthine

溶媒

DMF

反応条件

後処理

1. 1
   温度heated to 80° C
2. 2
   workup.WAITthe solution was left at 80° C. for 6 hours
3. 3
   温度After cooling to 50° C.
4. 4
   その他the precipitate obtained
5. 5
   ろ過was filtered off with suction
6. 6
   洗浄washed well with water
7. 7
   その他dried under reduced pressure
8. 8
   その他The dry residue was crystallized from dioxane/methanol

実験手順

3.2 g (0.1315 mol) of sodium hydride were added in portions to a suspension of 30 g (0.1315 mol) of 3-phenylxanthine in 600 ml of DMF, the mixture was stirred at 25° C. for 30 minutes and then heated to 80° C. 27 g (0.1578 mol) of benzyl bromide were then added and the solution was left at 80° C. for 6 hours. After cooling to 50° C., the reaction mixture was poured into 2000 ml of ice-water, and the precipitate obtained was filtered off with suction, washed well with water and dried under reduced pressure. The dry residue was crystallized from dioxane/methanol.

出典