反应详情

温度

100 °C

Under an N2 atmosphere, 985 ml (7.07 mol) of triethylamine, 892 g (3.21 mol) of tetra-nbutylammonium chloride and 12.77 g (57 mmol) of Pd(OAc)2 are added to 815 g (2.8 mol) of 2-iodo-benzoic acid allylamide in 4.5 l of DMF, and heated to 100° C. After 4 h, cooling is effected to RT, and the mixture is partially concentrated by evaporation on a RE. The residue is partitioned between 5 l of water and 5 l of EtOAc, the water phase is separated and extracted twice with EtOAc. The organic phases are washed with water, 0.1 N HCl, water and brine, dried (Na2SO4) and concentrated by evaporation. Column chromatography (SiO2, EtOAc/toluene 1:1) and crystallisation from toluene yields 4-methyl-2H-isoquinolin-1-one; m.p. 175-176° C.

1. temperaturecooling
2. customis effected to RT
3. concentrationthe mixture is partially concentrated by evaporation on a RE
4. customThe residue is partitioned between 5 l of water and 5 l of EtOAc
5. customthe water phase is separated
6. extractionextracted twice with EtOAc
7. washThe organic phases are washed with water, 0.1 N HCl, water and brine
8. dry with materialdried (Na2SO4)
9. concentrationconcentrated by evaporation
10. customColumn chromatography (SiO2, EtOAc/toluene 1:1) and crystallisation from toluene