反应详情

A mixture of methyl 3-fluoro-4-nitrobenzoate (5.8 g, 1 eq), N-Boc-1,3-diaminopropane (5.75 g, 1.1 eq) and potassium carbonate (8.04 g, 2 eq) in acetonitrile (200 ml) is heated under reflux for 2 hours then concentrated under reduced pressure at 40° C. The residue is taken up in dichloromethane (200 ml) and water (100 ml). After decantation and extractions, the combined organic phases are washed with salt water, dried over Na2SO4 then concentrated under reduced pressure at 40° C. The solid obtained is washed with petroleum ether and dried (10.2 g; 99% yield).

1. temperatureis heated
2. temperatureunder reflux for 2 hours
3. concentrationthen concentrated under reduced pressure at 40° C
4. extractionAfter decantation and extractions
5. washthe combined organic phases are washed with salt water
6. dry with materialdried over Na2SO4
7. concentrationthen concentrated under reduced pressure at 40° C
8. customThe solid obtained
9. washis washed with petroleum ether
10. customdried (10.2 g; 99% yield)