反应详情

0.300 g (0.9111 mmol) of 3-(1,6-dihydro-6-oxo-9H-purin-9-yl)propanoic acid, 4-nitrophenyl ester (AIT-0081) and 0.127 g (0.9111 mmol) of 3-amino-1-propane sulfonic acid were placed into a 10 ml round bottom flask with 2 ml of dimethylsulfoxide and a magnetic stirring bar. To this solution was added 0.100 g (0.988 mmol) of triethylamine and the solution immediately turned green. The solution was stirred at room temperature for five hours. Dimethylsulfoxide was removed in vacuo with gentle heating. 9 ml of acetone was added and the solution was triturated with methanol until homogeneous. No precipitate had formed. The solution was transferred to a 50 ml round bottom flask with 10 ml acetone and 5 ml methanol. Ether was added until just before the cloud point and the flask was placed into freezer overnight (<0° C.).

1. customDimethylsulfoxide was removed in vacuo with gentle heating
2. addition9 ml of acetone was added
3. customthe solution was triturated with methanol until homogeneous
4. customNo precipitate had formed
5. waitthe flask was placed into freezer overnight
6. custom(<0° C.)