Ethyl Acetate → 4-[6,7-Bis(methyloxy)quinolin-4-yl]-7-bromo-2,3,4,5-tetrahydro-1,4-benzoxazepine

참여 물질

역할	이름	HCID	투입량
반응물	Ethyl Acetate	HCID 8857	—
반응물	Potassium Carbonate	HCID 11430	—
반응물	4-Chloro-6,7-dimethoxyquinoline	HCID 459610	—
반응물	7-Bromo-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochloride	HCID 66820137	—
용매	1-Methylpyrrolidine	HCID 8454	—
생성물	4-[6,7-Bis(methyloxy)quinolin-4-yl]-7-bromo-2,3,4,5-tetrahydro-1,4-benzoxazepine	HCID 66819980	17%

반응 조건

온도	160 °C

반응 단계

A mixture of 7-bromo-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochloride (300 mg, 1.13 mmol), 4-chloro-6,7-dimethoxyquinoline (253 mg, 1.13 mmol), and potassium carbonate (470 mg, 3.40 mmol) in N-methylpyrrolidine (2 mL) was stirred at 160° C. for 17 h. Ethyl acetate (75 mL) was added and the mixture was washed with water (3×25 mL) and brine (25 mL), dried over sodium sulfate, and concentrated. Column chromatography on silica (dichloromethane:methanol 95:5) afforded 4-[6,7-bis(methyloxy)quinolin-4-yl]-7-bromo-2,3,4,5-tetrahydro-1,4-benzoxazepine (80 mg). MS (EI) for C20H19BrN2O3: 416 (MH+).

출처 및 근거

DOI	10.6084/m9.figshare.5104873.v1
특허 번호	US08648066B2
출처 데이터셋	uspto-grants-2014_02
ORD ID	ord-0f6eff0172b3404281ea183c831fa07d
출처 메모	uspto-grants-2014_02