Triethylamine → 4-amino-3-nitro-N-(6-trifluoromethylpyridin-3-yl)-benzamide

関与物質

役割	名称	HCID	仕込み量
反応物	Triethylamine	HCID 8471	—
反応物	Benzoic acid, 4-amino-3-nitro-	HCID 74115	—
反応物	5-Amino-2-(trifluoromethyl)pyridine	HCID 2737744	—
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	—
溶媒	Dimethylformamide	HCID 6228	—
生成物	4-amino-3-nitro-N-(6-trifluoromethylpyridin-3-yl)-benzamide	HCID 66966225	—

反応手順

To a solution of 6-trifluoromethylpyridin-3-ylamine (1.0 g, 6.17 mmol) and 4-amino-3-nitrobenzoic acid (1.12 g, 6.17 mmol) in DMF (25 mL) was added HATU (3.5 g, 9.23 mmol) followed by NEt3 (1.77 ml, 9.23 mmol). The reaction mixture was stirred at ambient temperature overnight. The reaction was quenched with water and extracted with EtOAc. The organic layer was washed with water, brine, dried with MgSO4, and filtered. The solvent was removed under reduced pressure and the residue was purified by flash chromatography using a heptane/EtOAc (1:1 then followed by 100% EtOAc) to give 4-amino-3-nitro-N-(6-trifluoromethylpyridin-3-yl)-benzamide as a red solid.

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US08222248B2
出典データセット	uspto-grants-2012_07
ORD ID	ord-6e0a824592ba4869a281ddcafb8f8b7b
出典メモ	uspto-grants-2012_07