反应详情

温度

110 °C

A solution of 6-chloro-3,3-dimethyl-2,3-dihydro-pyrrolo[3,2-c]pyridine-1-carboxylic acid tert-butyl ester (116 mg, 0.41 mmol), N-methylaniline (89 μL, 0.82 mmol), RuPhos (20 mg, 0.041 mmol), chloro(2-dicyclohexylphosphino-2′,6′-di-iso-propoxy-1,-1′-biphenyl)[2-(2-aminoethylphenyl)palladium(II), methyl-tert-butylether adduct (33 mg, 0.041 mmol) and NaOtBu (99 mg, 1.8 mmol) in toluene (2 mL) was evacuated and flushed with nitrogen. The mixture was stirred at 110° C. for 5 h. The mixtures was allowed to cool and then partitioned between EtOAc and water. The organic extract was washed with brine, dried (Na2SO4) and evaporated in vacuo. Chromatography (SiO2; gradient elution with 5-20% EtOAc in petrol) gave the title compound (112 mg, 56%) as a colourless solid. MS: [M+H]+=354.

1. customflushed with nitrogen
2. temperatureto cool
3. custompartitioned between EtOAc and water
4. extractionThe organic extract
5. washwas washed with brine
6. dry with materialdried (Na2SO4)
7. customevaporated in vacuo
8. washChromatography (SiO2; gradient elution with 5-20% EtOAc in petrol)