Methanamine, N-methoxy-, hydrochloride (1:1) → HCID 178502683、化合物

関与物質

役割	名称	HCID	仕込み量
反応物	Methanamine, N-methoxy-, hydrochloride (1:1)	HCID 81138	—
反応物	Diisopropylethylamine	HCID 81531	—
反応物	Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)	HCID 9886157	—
反応物	HCID 178524767	HCID 178524767	—
溶媒	Dimethylformamide	HCID 6228	—
溶媒	Ethyl Acetate	HCID 8857	—
生成物	HCID 178502683	HCID 178502683	—

反応手順

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.

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US08846698B2
出典データセット	uspto-grants-2014_09
ORD ID	ord-1240e203e19144038d94a0a8e0b1e77a
出典メモ	uspto-grants-2014_09