反应详情

温度

70 °C

A mixture of 72 mg (0.44 mMol) 2-amino-4,6-dichloropyrimidine, 143 mg (0.40 mMol) 6-hydroxy-benzo[d]isothiazole-3-carboxylic acid (4-fluoro-3-trifluoromethyl-phenyl)-amide and 280 mg (1.32 mMol) K3PO4 in 2 ml NMP is stirred for 6 h at 70° C. Then the mixture is diluted with EtOAc and water, the aq. layer separated off and extracted twice with EtOAc. The organic phases are washed twice with water and brine, dried (Na2SO4) and concentrated. Chromatography (Combi Flash; CH2Cl2→CH2Cl2/EtOH 9:1) gives the title compound: MS: [M−1]=482/484; TLC(CH2Cl2): Rf=0.12.

1. customthe aq. layer separated off
2. extractionextracted twice with EtOAc
3. washThe organic phases are washed twice with water and brine
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated