反应详情

Condensation of 306 and 72 was carried out in accord with the procedure described in step 6 of example 1 except 72 was used in place of 28 and 306 was used in place of 22. The crude product was purified by SiO2 chromatography eluting with a DCM/MeOH gradient (500:5 to 500:8) to afford 0.11 g (31.9%) of N-(3-(tert-butyldimethylsilyloxy)-1-(3,4-difluorophenyl)propyl)-2-(isopropylamino)-5,6-dihydropyrido[3,4-d]pyrimidine-7(8H)-carboxamide (308). The silyl group was removed with TBAF in accord with the procedure described in step 5 of example 42. The product was purified by SiO2 chromatography eluting with a DCM/MeOH gradient (500:15-500:25) to afford 0.010 g (12.8%) of I-77: MS m/z (APCI-pos) M+1=406.

1. customThe crude product was purified by SiO2 chromatography
2. washeluting with a DCM/MeOH gradient (500:5 to 500:8)