FC(F)(F)C(O)=O.[Cl:8][C:9]1[N:10]=[C:11]([N:18]2[CH2:23][CH2:22][O:21][CH2:20][CH2:19]2)[C:12]2[CH2:17][NH:16][CH2:15][C:13]=2[N:14]=1.Cl.[CH3:25][C:26]([CH3:28])=O.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>C1COCC1.C(O)(=O)C>[Cl:8][C:9]1[N:10]=[C:11]([N:18]2[CH2:19][CH2:20][O:21][CH2:22][CH2:23]2)[C:12]2[CH2:17][N:16]([CH:26]([CH3:28])[CH3:25])[CH2:15][C:13]=2[N:14]=1To a stirred solution of 4-(2-chloro-6,7-dihydro-5H-pyrrolo[3,4-d]pyrimidin-4-yl)morpholine (intermediate 20) as a HCl salt (455 mg, 1.6 mmol) in anhydrous THF (5 ml) was added anhydrous acetone (500 μl) and glacial acetic acid (two drops). The reaction was stirred at RT for 30 minutes after which time sodium triacetoxyborohydride (696 mg, 3.3 mmol) was added. After stirring for a further 2 hours at RT the reaction was partitioned between water and DCM. The aqueous phase was extracted into DCM and the organic extracts were combined and concentrated in vacuo to afford the title compound as a brown oil which was used without further purification.
Wird geladen…
