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), 2-methyl-phenol (38 mg, 0.42 mmol), 2-di-tert-butylphosphino-2′,4′,6′-triisopropylbiphenyl (tBuXPhos) (5 mg, 0.01 mmol), Pd(OAc)2 (1.6 mg, 0.007 mmol) and potassium phosphate (150 mg, 0.70 mmol) in toluene (2 mL) was evacuated and flushed with nitrogen. The mixture was stirred at 110° C. overnight then were 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 0-10% EtOAc in petrol) gave title compound (89 mg) {MS: [M+H]+=355} as an inseparable mixture with starting material.

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 0-10% EtOAc in petrol)