反応 #10530

反応方程式

3,4-dihydro-2H-pyran

2,6-Dichloro-9H-purine

4-toluenesulphonic acid monohydrate

sodium hydrogen carbonate

→

title compound

2,6-Dichloro-9-(tetrahydro-2H-pyran-2-yl)-9H-purine

溶媒

water

ethyl acetate

ethyl acetate

反応条件

後処理

1. 1
   温度The reaction mixture was cooled to room temperature
2. 2
   その他The organic layer was separated
3. 3
   洗浄washed sequentially with water and brine
4. 4
   乾燥dried over anhydrous magnesium sulphate
5. 5
   ろ過filtered
6. 6
   その他the solvent removed under reduced pressure
7. 7
   その他The residue was azeotroped with pentane (×2)

実験手順

2,6-Dichloro-9H-purine (20 g, 0.11 mol) and 4-toluenesulphonic acid monohydrate (0.2 g) were dissolved in ethyl acetate (300 ml), the mixture heated to 50° C. and a solution of 3,4-dihydro-2H-pyran (12.6 ml, 0.14 mol) in ethyl acetate (50 ml) added slowly over 30 minutes. The reaction mixture was cooled to room temperature, water (100 ml) added and the pH of the solution adjusted to 7 by addition of a saturated aqueous solution of sodium hydrogen carbonate. The organic layer was separated, washed sequentially with water and brine, dried over anhydrous magnesium sulphate, filtered and the solvent removed under reduced pressure. The residue was azeotroped with pentane (×2) to afford the title compound as a slightly impure white solid (30.9 g).

出典