Acetonitrile → 6-chloro-2-[1-(2-chlorophenyl)-3-trifluoromethyl-1H-pyrazol-5-yl]-8-methyl-4H-3,1-benzoxazine-4-one

To a mixture of 1.0 g of 1-(2-chlorophenyl)-3-trifluoromethyl-1H-pyrazole-5-carbonyl chloride and 10 ml of acetonitrile was added 0.60 g of 2-amino-5-chloro-3-methylbenzoic acid, and the resulting mixture was stirred at room temperature for 10 minutes. To the mixture, 0.46 ml of triethylamine was added. After the mixture was stirred at room temperature for 20 minutes, 0.92 ml of triethylamine was further added thereto. After the mixture was stirred at room temperature for 20 minutes, 0.28 ml of methanesulfonyl chloride was added thereto and the mixture was stirred at room temperature for 3 hours. The reaction mixture was filtered, and the resulting filtrate was concentrated under reduced pressure. The resulting residue was subjected to silica gel column chromatography to obtain 0.98 g of 6-chloro-2-[1-(2-chlorophenyl)-3-trifluoromethyl-1H-pyrazol-5-yl]-8-methyl-4H-3,1-benzoxazine-4-one of the formula:

1. stirringAfter the mixture was stirred at room temperature for 20 minutes
2. stirringAfter the mixture was stirred at room temperature for 20 minutes
3. stirringthe mixture was stirred at room temperature for 3 hours
4. filtrationThe reaction mixture was filtered
5. concentrationthe resulting filtrate was concentrated under reduced pressure

ORD 기록

ord-dca1628bfaff4eff901ad52175a991b7

출처 데이터셋

uspto-grants-2011_06

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07968573B2