反应详情

温度

150 °C

In a sealed tube, a mixture of 8-chloro-6-(2,4-dichloro-phenyl)-imidazo[1,2-a]pyridine-7-carbonitrile (20 mg, 0.062 mmol) and isobutylamine (0.037 mL, 0.37 mmol) was heated at 150° C. for 14 h. The reaction mixture was cooled to RT, poured into AcOEt (5 mL) and washed with a 2.0 M Na2CO3 solution in water (2×2 mL). The organic layer was dried over Na2SO4, filtered and evaporated. The residue was purified by Combi-Flash Companion™ (Isco Inc.) column chromatography (SiO2; gradient elution, [hexane/DCM 1:1]/TBME 95:5→8:2) to yield the title compound (19.1 mg, 0.053 mmol, 85%) as a reddish solid. MS: 359 [M+1]+; HPLC: AtRet=2.61; TLC: RF 0.64 (hexane/DCM/TBME 1:1:2).

1. temperatureThe reaction mixture was cooled to RT
2. washwashed with a 2.0 M Na2CO3 solution in water (2×2 mL)
3. dry with materialThe organic layer was dried over Na2SO4
4. filtrationfiltered
5. customevaporated
6. customThe residue was purified by Combi-Flash Companion™ (Isco Inc.) column chromatography (SiO2; gradient elution, [hexane/DCM 1:1]/TBME 95:5→8:2)