反应详情

A mixture of 294 mg (0.91 mMol) 6-hydroxy-benzo[d]isoxazole-3-carboxylic acid (3-trifluoromethyl-phenyl)-amide (Step 1.3), 149 mg (1.00 mMol) 2,4-dichlorpyrimidine and 426 mg (2.0 mMol) K3PO4 in 5 ml NMP is stirred for 20 h at rt. The reaction mixture is diluted with CH2Cl2 and 5% citric acid in water, the aq. phase separated off and extracted with CH2Cl2. The organic layers are washed with water and brine, dried (Na2SO4) and concentrated. Column chromatography (SiO2; CH2Cl2→CH2Cl2/EtOAc 99:1) gives the title compound: MS: [M+1]+=435; TLC(CH2Cl2/EtOAc 49:1): Rf=0.66.

1. customthe aq. phase separated off
2. extractionextracted with CH2Cl2
3. washThe organic layers are washed with water and brine
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated