反应详情

Combine formic acid (98-100%; 0.30 mL, 8 mmol) and 2-benzylaminoethanol (1.21 g, 8 mmol) and cool the resulting mixture with an ice bath. Add 2-bromo-1-(2-chloro-4-fluoro-phenyl)ethanone (1.0 g, 4 mmol); heat the mixture to reflux; and stir at that temperature for 20 h. Dilute the mixture with DCM and wash with saturated aqueous Na2CO3 solution. Dry organic phases over MgSO4; filter; collect the filtrate; and concentrate under reduced pressure. Purify via flash column chromatography eluting with a gradient of 0-20% methyl tertiary-butyl ether in hexanes. Combine the product fractions and remove the solvents under reduced pressure to give the title compound as a yellow oil (1.22 g, 43%). MS (m/z): 306 (M+1).

1. temperatureheat the mixture
2. temperatureto reflux
3. washwash with saturated aqueous Na2CO3 solution
4. filtrationfilter
5. customcollect the filtrate
6. concentrationand concentrate under reduced pressure
7. customPurify via flash column chromatography
8. washeluting with a gradient of 0-20% methyl tertiary-butyl ether in hexanes
9. customCombine the product fractions and remove the solvents under reduced pressure