1H-1,2,4-Triazole → (5-Methanesulfonyl-2-[1,2,4]triazol-1-yl-phenyl)-[4-(4-trifluoromethyl-phenyl)-piperazin-1-yl]-methanone

https://huagongshe.com/ko/reaction/32768

참여 물질

역할	이름	HCID	투입량
반응물	1H-1,2,4-Triazole	HCID 9257	—
반응물	Potassium Phosphate, Tribasic	HCID 62657	—
반응물	trans-N,N'-dimethyl-1,2-cyclohexanediamine	HCID 2733821	—
반응물	(2-Iodo-5-methanesulfonyl-phenyl)-[4-(4-trifluoromethyl-phenyl)-piperazin-1-yl]-methanone	HCID 59793691	—
촉매	Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)	HCID 24350	—
용매	Dimethylformamide	HCID 6228	—
생성물	(5-Methanesulfonyl-2-[1,2,4]triazol-1-yl-phenyl)-[4-(4-trifluoromethyl-phenyl)-piperazin-1-yl]-methanone	HCID 68838801	6.7%

반응 조건

온도	120 °C

반응 단계

In a tube were added successively (2-Iodo-5-methanesulfonyl-phenyl)-[4-(4-trifluoromethyl-phenyl)-piperazin-1-yl]-methanone (compound CK, 0.1 g, 0.19 mmol), 1,2,4-triazole (11 mg, 0.155 mmol), potassium phosphate (71 mg, 0.326 mmol), CuI (7 mg, 0.037 mmol), (1R,2R)-diaminomethylcyclohexane (2.3 mg, 0.015 mmol) and DMF (1 ml). The mixture was heated under argon at 120° C. for 24 hours. The reaction mixture was cooled to room temperature and quenched with water/dichloromethane. The aqueous layer was extracted twice with dichloromethane. The organic layers were combined, dried over Na2SO4, filtered and the solvent was removed in vacuo. The crude oil was chromatographed over silicagel: eluent: heptane/ethylacetate: 0-100% to provide the title compound as a light grey solid (5 mg, 6%), MS (m/e): 480.4 (M+H, 100%)

출처 및 근거

DOI	10.6084/m9.figshare.5104873.v1
특허 번호	US07427612B2
출처 데이터셋	uspto-grants-2008_09
ORD ID	ord-95f81d0e77d14d0099b96b00ce253733
출처 메모	uspto-grants-2008_09