反应详情

温度

100 °C

Intermediate 13 (0.0432 mol) was added at room temperature to phosphoryl chloride (150 ml). The mixture was stirred at 100° C. for 3 hours then brought to room temperature. The solvent was evaporated till dryness. The residue was taken up in DCM. The solvent was evaporated. The residue was taken up in DCM. The mixture was poured out into ice water, neutralized with K2CO3 solid and extracted with DCM. The organic layer was separated, washed with water, dried (MgSO4), filtered and the solvent was evaporated. The residue was crystallized from CH3CN. The precipitate was filtered off and dried under a vacuo, yielding 15.5 g (87%) of intermediate 14. The mother layer was purified by column chromatography over silica gel (eluent: toluene/EtOAc; 9317; 15-40 μm). The pure fractions were collected and the solvent was evaporated. The residue (0.7 g, 4%) was crystallized from 2-propanone. The precipitate was filtered off and dried under a vacuo, yielding 0.5 g (3%) of [2-chloro-4-(3-chlorophenyl)-6-quinazolinyl](4-methoxyphenyl)-methanone (intermediate 14), mp. 175° C.

1. customthen brought to room temperature
2. customThe solvent was evaporated till dryness
3. customThe solvent was evaporated
4. additionThe mixture was poured out into ice water
5. extractionextracted with DCM
6. customThe organic layer was separated
7. washwashed with water
8. dry with materialdried (MgSO4)
9. filtrationfiltered
10. customthe solvent was evaporated
11. customThe residue was crystallized from CH3CN
12. filtrationThe precipitate was filtered off
13. customdried under a vacuo