Tetrahydrofuran → 3-bromo-N-[4,6-dibromo-2-(N,N'-dimethylhydrazinocarbonyl)phenyl]-1-(3-chloro-2-pyridinyl)-1H-pyrazole-5-carboxamide

https://huagongshe.com/ja/reaction/252003

関与物質

役割	名称	HCID	仕込み量
反応物	Tetrahydrofuran	HCID 8028	—
反応物	1,2-Dimethylhydrazine dihydrochloride	HCID 9380	—
反応物	Potassium Carbonate	HCID 11430	—
反応物	2-[5-bromo-2-(3-chloro-pyridin-2-yl)-2H-pyrazol-3-yl]-6,8-dibromo-benzo[d][1,3]oxazin-4-one	HCID 59200307	—
触媒	Water	HCID 962	—
溶媒	Water	HCID 962	—
生成物	3-bromo-N-[4,6-dibromo-2-(N,N'-dimethylhydrazinocarbonyl)phenyl]-1-(3-chloro-2-pyridinyl)-1H-pyrazole-5-carboxamide	HCID 57780381	76.8%

反応手順

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 0.60 g of 2-[3-bromo-1-(3-chloro-2-pyridinyl)-1H-pyrazol-5-yl]-6,8-dibromo-4H-3,1-benzoxazine-4-one. The resulting mixture was stirred at room temperature for 19 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 0.51 g of 3-bromo-N-[4,6-dibromo-2-(N,N′-dimethylhydrazinocarbonyl)phenyl]-1-(3-chloro-2-pyridinyl)-1H-pyrazole-5-carboxamide of the formula:

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US07867949B2
出典データセット	uspto-grants-2011_01
ORD ID	ord-543b30e4a93149fc88c3b5f44572d0fb
出典メモ	uspto-grants-2011_01