Dimethylformamide → n-[6-Chloro-4-(2-chloro-phenyl)-pyridin-3-yl]-2-(3-chloro-5-difluoromethoxy-phenyl)-n-methyl-isobutyramide

関与物質

役割	名称	HCID	仕込み量
反応物	Dimethylformamide	HCID 6228	—
反応物	Acetic acid, 2-chloro-2,2-difluoro-, ethyl ester	HCID 67843	—
反応物	HCID 86597668	HCID 86597668	—
溶媒	Water	HCID 962	—
生成物	n-[6-Chloro-4-(2-chloro-phenyl)-pyridin-3-yl]-2-(3-chloro-5-difluoromethoxy-phenyl)-n-methyl-isobutyramide	HCID 87304771	49%

反応条件

温度	65 °C

反応手順

To a solution of 0.700 g (1.56 mmol) N-[6-chloro-4-(2-chloro-phenyl)-pyridin-3-yl]-2-(3-chloro-5-hydroxy-phenyl)-N-methyl-isobutyramide in 10 ml N,N-Dimethylformamide 0.215 g (1.56 mmol) K2CO3 and 0.2 ml (1.56 mmol) ethyl chlordifluoroacetate was added and the resulting suspension heated at 65° C. for 15 h. After cooling to ambient temperature, the reaction mixture was poured into 75 ml water and extracted three times with 80 ml CH2Cl2. The combined organic solvents were dried (Na2SO4), filtered and evaporated. The residue was purified by flash-chromatography (SiO2, CH2Cl2/ethyl acetate 4:1) to give 0.38 g (49%) of the title compound as a white solid.

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US07939533B2
出典データセット	uspto-grants-2011_05
ORD ID	ord-6649c87f912c42efa9ad52606b63f7a8
出典メモ	uspto-grants-2011_05