Triethylamine → benzoic acid N'-[2-(2-sec-butyl-phenoxy)-acetyl]-N'-isopropyl-hydrazide

関与物質

役割	名称	HCID	仕込み量
反応物	Triethylamine	HCID 8471	—
反応物	1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide	HCID 15908	—
反応物	1-Benzoyl-2-isopropylhydrazine	HCID 18869	—
反応物	1-Hydroxybenzotriazole	HCID 75771	—
反応物	(2-Sec-butylphenoxy)acetic acid	HCID 3365714	—
溶媒	Dimethylformamide	HCID 6228	—
生成物	benzoic acid N'-[2-(2-sec-butyl-phenoxy)-acetyl]-N'-isopropyl-hydrazide	HCID 11566858	36.4%

反応手順

A solution of (2-sec-butyl-phenoxy)-acetic acid (193 mg, 0.93 mmol), and benzoic acid N′-isopropyl-hydrazide (150 mg, 0.842 mmol) in DMF (5 ml), was treated with triethylamine (0.352 ml, 2.52 mmol), HOBT (136 mg, 1.00 mmol), and EDCI (194 mg, 1.00 mmol) for 12 hours at room temperature. The reaction mixture was partitioned between 1N HCl and DCM. The organic layer was successively washed with 1N NaOH and brine, then dried over sodium sulfate, filtered, and concentrated. The crude was absorbed on silica and purified on a silica gel column with 50% ethyl acetate/hexanes to afford the product as a white solid (113 mg, 33%). MS m/e 369.32 (M+H+)

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US07317125B2
出典データセット	uspto-grants-2008_01
ORD ID	ord-fcb937a1d1344f42b2833a0eaa607652
出典メモ	uspto-grants-2008_01