Methanamine, N-methoxy-, hydrochloride (1:1) → HCID 178502683, 화합물

참여 물질

역할	이름	HCID	투입량
반응물	Methanamine, N-methoxy-, hydrochloride (1:1)	HCID 81138	—
반응물	Diisopropylethylamine	HCID 81531	—
반응물	Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)	HCID 9886157	—
반응물	HCID 178524767	HCID 178524767	—
용매	Dimethylformamide	HCID 6228	—
용매	Ethyl Acetate	HCID 8857	—
생성물	HCID 178502683	HCID 178502683	—

반응 단계

5-Bromo-6-hydroxy-nicotinic acid (Preparation 238, 4 g, 18.4 mmol), HATU (13.95 g, 36.71 mmol), O,N-Dimethyl-hydroxylamine hydrochloride (2.15 g, 22.02 mmol) and DIPEA (15.82 mL, 91.75 mmol) were taken in anhydrous DMF (30 mL). The mixture was stirred at room temperature for 16 hours. The reaction mixture was diluted with EtOAc (150 mL), washed with saturated aq. Na2CO3 (2×50 mL), water (4×30 mL), brine (30 mL), dried (Na2SO4) and evaporated in vacuo. The crude mixture was purified by column chromatography on silica gel (gradient of EtOAc:Hex 4:6 to 6:4) to afford the title compound as light yellow sticky solid in 38%, 1.8 g.

출처 및 근거

DOI	10.6084/m9.figshare.5104873.v1
특허 번호	US08846698B2
출처 데이터셋	uspto-grants-2014_09
ORD ID	ord-1240e203e19144038d94a0a8e0b1e77a
출처 메모	uspto-grants-2014_09