반응 #10534

반응 방정식

water

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

potassium cyanide

→

title compound

수율 95.1%

6-[(2,2-Diphenylethyl)amino]-9-(tetrahydro-2H-pyran-2-yl)-9H-purine-2-carbonitrile

수율 95.1%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   온도The mixture was cooled to room temperature
2. 2
   여과The resultant solid was filtered
3. 3
   세척washed several times with water
4. 4
   workup.DISSOLUTIONThe solid was then dissolved in dichloromethane
5. 5
   세척the solution washed with water
6. 6
   건조dried with anhydrous magnesium sulphate
7. 7
   여과filtered
8. 8
   기타the solvent removed under reduced pressure
9. 9
   기타The residue was azeotroped with diethyl ether (twice)

실험 절차

A solution of N-(2,2-diphenylethyl)-2-(methylsulfonyl)-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine (Preparation 4) (20.1 g, 42.1 mmol) in dry N,N-dimethylformamide (100 ml) was treated with potassium cyanide (5.5 g, 84.6 mmol) and the mixture heated at 120° C. for 24 hours under a nitrogen atmosphere. The mixture was cooled to room temperature, poured into water (1000 ml) and stirring continued for a further 1 hour. The resultant solid was filtered and washed several times with water. The solid was then dissolved in dichloromethane and the solution washed with water, dried with anhydrous magnesium sulphate, filtered and the solvent removed under reduced pressure. The residue was azeotroped with diethyl ether (twice) to afford the title compound as an oil (17 g).

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