反应详情

温度

120 °C

A mixture of N′-(2,6-dichloro-4-phenyl-quinoline-3-carbonyl)-hydrazinecarboxylic acid 9H-fluoren-9-ylmethyl ester (130 mg, 211 μmol, Eq: 1.00), piperidine (180 mg, 209 μl, 2.11 mmol, Eq: 10) and triethylamine (64.1 mg, 88.2 μl, 633 μmol, Eq: 3) in DMF (2 ml) was heated to 120° C. for 20 min in a microwave. Water was added and the mixture was extracted with ethyl acetate (3×). The combined extracts were washed with water and brine, dried with Na2SO4 and evaporated. The remaining residue was purified by column chromatography (silica gel, DCM/EtOAc 9:1-4:1) to afford the title compound as light yellow solid (31 mg). MS (ESI): 381.2 (M+H)+.

1. extractionthe mixture was extracted with ethyl acetate (3×)
2. washThe combined extracts were washed with water and brine
3. dry with materialdried with Na2SO4
4. customevaporated
5. customThe remaining residue was purified by column chromatography (silica gel, DCM/EtOAc 9:1-4:1)