反应详情

温度

80 °C

To a mixture of [3-amino-6-(2,4-dichloro-phenyl)-imidazo[1,2-a]pyridin-7-ylmethyl]-carbamic acid tert-butyl ester (100 mg, 0.25 mmol), tetrahydro-pyran-4-arboxylic acid (192 mg, 1.47 mmol) and DIPEA (0.52 mL, 2.95 mmol) in DMF (3 mL) was added HATU (560 mg, 1.47 mmol) at RT. The reaction mixture was heated at 80° C. and stirred for 24 h, then poured into AcOEt (50 mL) and washed with a 2.0 M aqueous Na2CO3 solution (2×25 mL). The organic layer was dried over Na2SO4, filtered, and evaporated to dryness. The remaining residue was purified by Combi-Flash Companion™ (Isco Inc.) column chromatography (SiO2; gradient elution, DCM/MeOH 99:1→84:16) to yield the title compound (79.5 mg, 0.153 mmol, 62%). MS: 519 [M+1]+; HPLC: AtRet=1.49; TLC: RF 0.14 (DCM/MeOH 95:5).

1. washwashed with a 2.0 M aqueous Na2CO3 solution (2×25 mL)
2. dry with materialThe organic layer was dried over Na2SO4
3. filtrationfiltered
4. customevaporated to dryness
5. customThe remaining residue was purified by Combi-Flash Companion™ (Isco Inc.) column chromatography (SiO2; gradient elution, DCM/MeOH 99:1→84:16)