Potassium Carbonate → 1-(4-Chloro-2-(3-methyl-1H-pyrazol-1-yl)phenyl)-2,2,2-trifluoroethanol

https://huagongshe.com/reaction/1620847

참여 물질

역할	이름	HCID	투입량
반응물	Potassium Carbonate	HCID 11430	—
반응물	trans-N,N'-dimethyl-1,2-cyclohexanediamine	HCID 2733821	—
반응물	1-(4-Chloro-2-iodo-phenyl)-2,2,2-trifluoro-ethanol	HCID 66743638	—
반응물	HCID 178428694	HCID 178428694	—
촉매	Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)	HCID 24350	—
용매	Toluene	HCID 1140	—
용매	Ethyl Acetate	HCID 8857	—
생성물	1-(4-Chloro-2-(3-methyl-1H-pyrazol-1-yl)phenyl)-2,2,2-trifluoroethanol	HCID 25212415	33%

반응 조건

온도	130 °C

반응 단계

1-(4-Chloro-2-iodo-phenyl)-2,2,2-trifluoro-ethanol (0.840 g, 2.5 mmol), 3-methyl pyrazole (0.230 g, 2.8 mmol), CuI (0.190 g, 1.0 mmol), K2CO3 (0.863 g, 6.25 mmol), (1R,2R)-N,N′-dimethyl-cyclohexane-1,2-diamine (0.071 g, 0.5 mmol) and toluene (10 ml) were combined in a 20 ml pressure tube, and the mixture was heated at 130° C. (oil bath temperature) for 12 h. The mixture was diluted with ethyl acetate and washed with H2O (2×20 ml), brine, and dried over sodium sulfate. Removal of solvent gave a crude product, which was purified by ISCO column chromatography using 5-10% ethyl acetate in hexane as solvent to afford 1-[4-chloro-2-(3-methyl-pyrazol-1-yl)-phenyl]-2,2,2-trifluoro-ethanol (240 mg).

출처 및 근거

DOI	10.6084/m9.figshare.5104873.v1
특허 번호	US08772482B2
출처 데이터셋	uspto-grants-2014_07
ORD ID	ord-cd07556e158448af8b214f837a004e02
출처 메모	uspto-grants-2014_07