反应详情

The crude 6-azido-4-(quinolin-6-yloxy)-pyrimidine (36.4 mMol) in 324 ml of THF/acetic acid 4:1 is hydrogenated in the presence of 6 g Pd/C (10% Engelhard 4505). Then the catalyst is filtered off and the filtrate concentrated in vacuuo. The residue is put to pH 10 by addition of sat. Na2CO3 solution and extracted 3× with EtOAC. The organic phases are washed with water and brine, dried (Na2SO4) and after addition of 40 g of SiO2 concentrate in vacuo. The resulting powder is put on top of a SiO2 chromatography column and the title compound eluated with EtOAc: MS: [M+1]+=243.

1. filtrationThen the catalyst is filtered off
2. concentrationthe filtrate concentrated in vacuuo
3. additionThe residue is put to pH 10 by addition of sat. Na2CO3 solution
4. extractionextracted 3× with EtOAC
5. washThe organic phases are washed with water and brine
6. dry with materialdried (Na2SO4)
7. additionafter addition of 40 g of SiO2
8. concentrationconcentrate in vacuo