反应详情

300 mg (0.938 mMol) 6-(2-chloro-pyrimidin-4-yloxy)-benzo[d]isoxazole-3-carboxylic acid ethyl ester in 3 ml DMF and 262 μl (1.88 mMol) Et3N are hydrogenated in presence of 120 mg Pd/C (10%; Engelhard 4505). The catalyst is filtered off, the filtrate concentrated, the residue re-dissolved in EtOAc and water, the aq. layer separated off and extracted with EtOAc. The organic layers are washed with water and brine, dried (Na2SO4) and concentrated. Chromatography (Combi Flash; hexane/EtOAc 9:1→4:1) gives the title compound: MS: [M+1]+=286; TLC(hexane/EtOAc 1:1): Rf=0.30.

1. filtrationThe catalyst is filtered off
2. concentrationthe filtrate concentrated
3. dissolutionthe residue re-dissolved in EtOAc
4. customwater, the aq. layer separated off
5. extractionextracted with EtOAc
6. washThe organic layers are washed with water and brine
7. dry with materialdried (Na2SO4)
8. concentrationconcentrated