1,10-Phenanthroline → 1-{6-[(3-Cyclobutyl-2,3,4,5-tetrahydro-1H-3-benzazepin-7-yl)oxy]-3-pyridinyl}-5-methyl-2-pyrrolidinone

https://huagongshe.com/ko/reaction/222735

참여 물질

역할	이름	HCID	투입량
반응물	1,10-Phenanthroline	HCID 1318	—
반응물	Cesium carbonate	HCID 10796	—
반응물	5-Methyl-2-pyrrolidone	HCID 66055	—
반응물	1H-3-Benzazepine, 3-cyclobutyl-2,3,4,5-tetrahydro-7-[(5-iodo-2-pyridinyl)oxy]-	HCID 57440294	—
촉매	Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)	HCID 24350	—
용매	1,4-Dioxane	HCID 31275	—
생성물	1-{6-[(3-Cyclobutyl-2,3,4,5-tetrahydro-1H-3-benzazepin-7-yl)oxy]-3-pyridinyl}-5-methyl-2-pyrrolidinone	HCID 10430564	50%

반응 조건

온도	175 °C

반응 단계

3-Cyclobutyl-7-[(5-iodo-2-pyridinyl)oxy]-2,3,4,5-tetrahydro-1H-3-benzazepine (E207) (294 mg, 0.7 mmol) 1,10 phenanthroline (38 mg, 0.2 mmol), 5-methyl-2-pyrrolidinone (139 mg 1.4 mmol) were dissolved in dioxane (2 ml). Copper(I) Iodide (39 mg, 0.2 mmol) and caesium carbonate (479 mg, 1.5 mmol) were added and the mixture heated in a microwave reactor at 175° C. for 15 minutes. The mixture was cooled and filtered through celite, washing through with dichloromethane. The filtrate was concentrated in vacuo and the crude material purified by column chromatography, eluting with dichloromethane through to a mixture of 0.880 ammonia:methanol:dichloromethane (1:9:90) to afford the title compound (137 mg); MS (ES+) m/e 392 [M+H]+.

출처 및 근거

DOI	10.6084/m9.figshare.5104873.v1
특허 번호	US08207331B2
출처 데이터셋	uspto-grants-2012_06
ORD ID	ord-3c0b5f00e5b047a28b1d01e07da96d6f
출처 메모	uspto-grants-2012_06