Tetrahydrofuran → 4-bromo-N-[4,6-dibromo-2-(N,N'-dimethylhydrazinocarbonyl)phenyl]-1-(3-chloro-2-pyridinyl)-1H-pyrrole-2-carboxamide

To a mixture of 0.42 g of N,N′-dimethylhydrazine dihydrochloride, five drops of water, 0.87 g of potassium carbonate and 10 ml of tetrahydrofuran was added 0.59 g of 6,8-dibromo-2-[4-bromo-1-(3-chloro-2-pyridinyl)-1H-pyrrol-2-yl]-4H-3,1-benzoxazine-4-one. The resulting mixture was stirred at room temperature for 2 hours. Water was poured into the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed successively with water and an aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The resulting residue was subjected to silica gel chromatography to obtain 0.52 g of 4-bromo-N-[4,6-dibromo-2-(N,N′-dimethylhydrazinocarbonyl)phenyl]-1-(3-chloro-2-pyridinyl)-1H-pyrrole-2-carboxamide of the formula:

1. extractionthe mixture was extracted with ethyl acetate
2. washThe organic layer was washed successively with water
3. dry with materialan aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate
4. concentrationconcentrated under reduced pressure

ORD 기록

ord-bda843301c224fc7b8683dd5bb097550

출처 데이터셋

uspto-grants-2011_01

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07867949B2