反应详情

温度

110 °C

A vessel containing 6-chloro-3,3-dimethyl-2,3-dihydro-pyrrolo[3,2-c]pyridine-1-carboxylic acid tert-butyl ester (100 mg, 0.35 mmol), aniline (64 μL, 0.71 mmol), 2-(dicyclohexylphosphino)-3,6-dimethoxy-2′-4′-6′-tri-1-propyl-1,1′-biphenyl (19 mg, 0.035 mmol), Pd2(dba)3 (16 mg, 0.018 mmol) and NaOtBu (51 mg, 0.53 mmol) in toluene (2 mL) was evacuated and flushed with nitrogen. The mixture was stirred at 110° C. overnight, then 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 50-100% EtOAc in petrol) gave the title compound (60 mg, 50%) as a colourless solid. MS: [M+H]+=340.

1. customwas evacuated
2. customflushed with nitrogen
3. temperatureto cool
4. custompartitioned between EtOAc and water
5. extractionThe organic extract
6. washwas washed with brine
7. dry with materialdried (Na2SO4)
8. customevaporated in vacuo
9. washChromatography (SiO2; gradient elution with 50-100% EtOAc in petrol)