تفاعل #10534

معادلة التفاعل

water

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

potassium cyanide

→

title compound

المردود 95.1%

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

المردود 95.1%

المذيبات

N,N-dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe mixture was cooled to room temperature
2. 2
   ترشيحThe resultant solid was filtered
3. 3
   غسيلwashed several times with water
4. 4
   workup.DISSOLUTIONThe solid was then dissolved in dichloromethane
5. 5
   غسيلthe solution washed with water
6. 6
   تجفيفdried with anhydrous magnesium sulphate
7. 7
   ترشيحfiltered
8. 8
   أخرىthe solvent removed under reduced pressure
9. 9
   أخرىThe residue was azeotroped with diethyl ether (twice)

الإجراء التجريبي

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).

المصدر