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HRID 642001作成日:2026年10月24日

Diethyl Ether → 1-(3-chloro-2-pyridinyl)-N-[2-methyl-6-[[(1-methylethyl)amino]carbonyl]phenyl]-3-(trifluoromethyl)-1H-pyrazole-5-carboxamide

https://huagongshe.com/ja/reaction/642001

反応式

関与物質

役割名称HCID仕込み量
反応物Diethyl EtherHCID 3283—
反応物IsopropylamineHCID 6363—
反応物2-[1-(3-chloro-2-pyridinyl)-3-trifluoromethyl-1H-pyrazol-5-yl]-8-methyl-4H-3,1-benzoxazine-4-oneHCID 23150348—
溶媒DichloromethaneHCID 6344—
生成物1-(3-chloro-2-pyridinyl)-N-[2-methyl-6-[[(1-methylethyl)amino]carbonyl]phenyl]-3-(trifluoromethyl)-1H-pyrazole-5-carboxamideHCID 1029858787.3%

反応手順

To a suspension of the benzoxazinone product of Step D (124 g, 300 mmol) in dichloromethane (500 mL) was added dropwise isopropylamine (76 mL, 900 mmol) at room temperature. The temperature of the reaction mixture rose and the suspension thinned during the addition. The reaction mixture was then warmed to reflux for 1.5 h. A new suspension formed. The reaction mixture was cooled to room temperature and diethyl ether (1.3 L) was added and the mixture stirred at room temperature overnight. The solids were collected and washed with ether. The solids were air-dried and then dried in vacuo at 90° C. for 5 h to yield 122 g of the title compound, a compound of the present invention, as a fluffy white solid, melting at 194-196° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07696232B2
出典データセットuspto-grants-2010_04
ORD IDord-9b0956bdbb524bb6984e301e131f6d20
出典メモuspto-grants-2010_04