反应详情

To a solution of 3-[4-(2,6-dioxo-1,3-dipropyl-2,3,6,7-tetrahydro 1H-purin-8-yl)-bicyclo-[2.2.2]oct-1-yl]-propionic acid(510m, 1.22 mmol) and HATU (1.1 eq, 1.34 mmol, 511 mg) in DMF (10 ml) was added Hunig's base (1.3 eq, 1.60 mmol, 205 mg). After the resulting suspension had been stirred for 1 h, excess ammonia (0.5 M in dioxane, 4.0 ml) was added and the mixture was stirred overnight (14 h). The solvent was removed in vacuo and the resulting residue was partitioned between CH2Cl2 (10 ml) and 1 N HCl (10 ml) with the aid of 2 ml MeOH to assist in the transfer and improve solubility. The aqueous phase was extracted with CH2C2 (2×10 ml), the combined organic phases were washed with 1 N HCl (2×10 ml), dried (MgSO4), filtered and evaporated in vacuo to give an off-white solid (455 mg, 90%). MS: 416 (MH+).

1. stirringthe mixture was stirred overnight (14 h)
2. customThe solvent was removed in vacuo
3. customthe resulting residue was partitioned between CH2Cl2 (10 ml) and 1 N HCl (10 ml) with the aid of 2 ml MeOH
4. extractionThe aqueous phase was extracted with CH2C2 (2×10 ml)
5. washthe combined organic phases were washed with 1 N HCl (2×10 ml)
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. customevaporated in vacuo