反应详情

温度

40 °C

Sodium hydride (79 mg (1.5 eq.) was added at 0° C. to a solution of 4-hydroxymethyl-cyclohexanol (3 g, 12 mmol, synthesised analogously to J. Org. Chem. 1994 59 p. 2748–2761) in DMF (30 ml). After 20 minutes, a solution of 4-chloro-6-methoxy-quinazoline (1.94 g, 10 mmol) in DMF (10 ml) was added and the reaction mixture was heated to 40° C. After a further 2 hours, the reaction mixture was concentrated to dryness. The residue was diluted with water (100 ml) and ethyl acetate (100 ml), the phases were separated and the aqueous phase was extracted twice using 50 ml of ethyl acetate each time. The combined organic phases were dried over MgSO4, filtered and concentrated to dryness by rotary evaporation. The residue was purified by column chromatography on silica gel (EtOAc/hexane 1/2).

1. customsynthesised analogously to J
2. waitAfter a further 2 hours
3. concentrationthe reaction mixture was concentrated to dryness
4. additionThe residue was diluted with water (100 ml) and ethyl acetate (100 ml)
5. customthe phases were separated
6. extractionthe aqueous phase was extracted twice
7. dry with materialThe combined organic phases were dried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated to dryness by rotary evaporation
10. customThe residue was purified by column chromatography on silica gel (EtOAc/hexane 1/2)