Water → (R)-2-(4-cyano-3,5-difluorophenylamino)-4-methylpentanamide

関与物質

役割	名称	HCID	仕込み量
反応物	Water	HCID 962	—
反応物	Diisopropylethylamine	HCID 81531	—
反応物	2,4,6-Trifluorobenzonitrile	HCID 737177	—
反応物	(R)-2-Amino-4-methylpentanamide hydrochloride	HCID 56776963	—
溶媒	Dimethyl Sulfoxide	HCID 679	—
溶媒	Ethyl Acetate	HCID 8857	—
生成物	(R)-2-(4-cyano-3,5-difluorophenylamino)-4-methylpentanamide	HCID 67509019	26.1%

反応手順

To a solution of 2,4,6-trifluorobenzonitrile (208 mg, 1.32 mmol) in DMSO (2 mL), a solution of D-leucine amide hydrochloride (220 mg, 1.32 mmol) and DIEA (0.688 mL, 3.96 mmol) in DMSO (5 mL) was added. After being stirred at room temperature for 18 h, water and EtOAc were added. The organic phase was separated, washed with water, dried over Na2SO4, concentrated in vacuo. The residue was purified by a silica gel column, eluted with 20-80% EtOAc in hexane to give (R)-2-(4-cyano-3,5-difluorophenylamino)-4-methylpentanamide (92 mg).

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US08846928B2
出典データセット	uspto-grants-2014_09
ORD ID	ord-71e08a4bb760452385e7a27395a1cdd3
出典メモ	uspto-grants-2014_09