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HRID 598447作成日:2026年10月24日

Methylamine → N-methyl-3-(4-nitrophenoxy)benzamide

https://huagongshe.com/ja/reaction/598447

反応式

関与物質

役割名称HCID仕込み量
反応物MethylamineHCID 6329—
反応物3-(4-Nitrophenoxy)benzoic acidHCID 767919—
反応物1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 2723939—
触媒Ni methylmorpholineHCID 131728719—
溶媒DichloromethaneHCID 6344—
生成物N-methyl-3-(4-nitrophenoxy)benzamideHCID 2361456948.2%

反応手順

A mixture of 4-(3-carboxyphenoxy)-1-nitrobenzene (3.72 g, 14.4 mmol), EDCI.HCl (3.63 g, 18.6 mmol), Ni-methylmorpholine (1.6 mL, 14.5 mmol) and methylamine (2.0 M in THF 8 mL, 16 mmol) in CH2Cl2 (45 mL) was stirred at room temp. for 3 d, then concentrated under reduced pressure. The residue was dissolved in EtOAc (50 mL) and the resulting mixture was extracted with a 1M HCl solution (50 mL). The aqueous layer was back-extracted with EtOAc (2×50 mL). The combined organic phases were washed with a saturated NaCl solution (50 mL), dried (Na2SO4), and concentrated under reduced pressure to give 4-(3-(N-methylcarbamoyl)phenoxy)-1-nitrobenzene as an oil (1.89 g).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07897623B2
出典データセットuspto-grants-2011_03
ORD IDord-4378fea5add54ce29dfdc319cee76cd5
出典メモuspto-grants-2011_03