反应详情

33 mg (0.13 mmol) spiro[piperidin-4,4′-pyrido[2,3-d][1,3]oxazin]-2′(1′H)-one hydrochloride, 40 mg (0.12 mmol) 7-methyl-5-(6-chloropyrimidin-4-yloxy)-2-(tetrahydro-2H-pyran-4-yl)-1H-benzo[d]imidazole and 70 μL (0.39 mmol) DIPEA in 2.0 mL DMF were stirred overnight at 60° C. The reaction mixture was poured onto ice water and the precipitate formed was suction filtered. The precipitate was dissolved and then purified by chromatography. The fractions containing product were combined and evaporated down i.vac. to leave the aqueous residue. This was neutralised with an aqueous NaHCO3 solution. The precipitate formed was suction filtered, washed and dried.

1. additionThe reaction mixture was poured onto ice water
2. customthe precipitate formed
3. filtrationfiltered
4. dissolutionThe precipitate was dissolved
5. custompurified by chromatography
6. additionThe fractions containing product
7. customevaporated down i.vac
8. customto leave the aqueous residue
9. customThe precipitate formed
10. filtrationfiltered
11. washwashed
12. customdried