반응 #10530

반응 방정식

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

용매

water

ethyl acetate

ethyl acetate

반응 조건

후처리

1. 1
   온도The reaction mixture was cooled to room temperature
2. 2
   기타The organic layer was separated
3. 3
   세척washed sequentially with water and brine
4. 4
   건조dried over anhydrous magnesium sulphate
5. 5
   여과filtered
6. 6
   기타the solvent removed under reduced pressure
7. 7
   기타The residue was azeotroped with pentane (×2)

실험 절차

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).

출처