反应详情

Add triethylamine drop wise (3 equiv) to a suspension of 1-(3-methyl-5-nitro-pyridin-2-yl)-piperazine; hydrochloride (6.91 g, 24.13 mmol) in DCM (120 mL). Add 2,6-difluorobenzoylchloride (1 equiv.) Stir the mixture at room temperature overnight. Add additional 2,6-difluorobenzoylchloride (1.6 mL) and triethylamine (1.5 equiv.) to run reaction to completion. Allow the reaction to stand overnight. Dilute with DCM and extract several times with water. Dry the organic layer over Na2S2O4, filter, and remove solvent under reduced pressure. Wash solid several times with hexane to obtain. 8.08 g of (2,6-difluoro-phenyl)-[4-(3-methyl-5-nitro-pyridin-2-yl)-piperazin-1-yl]-methanone (93% yield). ES+(m/z): 363 [M+1]

1. customreaction to completion
2. customthe reaction
3. extractionextract several times with water
4. dry with materialDry the organic layer over Na2S2O4
5. filtrationfilter
6. customremove solvent under reduced pressure
7. washWash solid several times with hexane
8. customto obtain