반응 #10533

반응 방정식

Oxone

N-(2,2-diphenylethyl)-2-(methylsulfanyl)-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine

sodium hydrogencarbonate

→

title compound

수율 75.7%

N-(2,2-Diphenylethyl)-2-(methylsulfonyl)-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine

수율 75.7%

용매

water

acetone

water

반응 조건

후처리

1. 1
   여과filtered
2. 2
   세척the residue washed with acetone
3. 3
   기타The acetone was removed from the filtrate under reduced pressure
4. 4
   추출the resulting aqueous residue extracted with ethyl acetate
5. 5
   세척The combined organic layers were washed with brine
6. 6
   건조dried with anhydrous magnesium sulphate
7. 7
   여과filtered
8. 8
   기타the solvent removed under reduced pressure
9. 9
   기타The residue was triturated with diethyl ether
10. 10
    여과filtered
11. 11
    세척washed with diethyl ether and pentane
12. 12
    기타dried

실험 절차

A solution of Oxone (trade mark) (potassium peroxymonosulphate) (44 g, 71.7 mmol) in water (200 ml) was added dropwise over 2 hours to a solution of N-(2,2-diphenylethyl)-2-(methylsulfanyl)-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine (Preparation 3) (25 g, 56.2 mmol) and sodium hydrogencarbonate (20 g, 238 mmol) in acetone (1000 ml) and water (250 ml). The resultant mixture was stirred at room temperature for 24 hours, filtered and the residue washed with acetone. The acetone was removed from the filtrate under reduced pressure and the resulting aqueous residue extracted with ethyl acetate and then dichloromethane. The combined organic layers were washed with brine, dried with anhydrous magnesium sulphate, filtered and the solvent removed under reduced pressure. The residue was triturated with diethyl ether, filtered, washed with diethyl ether and pentane and then dried to afford the title compound as a white solid (20.32 g).

출처