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HRID 517482作成日:2026年10月25日

Ethyl Acetate → 4-Chloro-N-{2-[4-(difluoromethoxy)phenyl]ethyl}-6-methoxy-1,3,5-triazin-2-amine

https://huagongshe.com/reaction/517482

反応式

関与物質

役割名称HCID仕込み量
反応物Ethyl AcetateHCID 8857—
反応物2,4-Dichloro-6-methoxy-3,5-triazineHCID 19267—
反応物DiisopropylethylamineHCID 81531—
反応物2-(4-(Difluoromethoxy)phenyl)ethan-1-amineHCID 4962292—
溶媒WaterHCID 962—
溶媒AcetonitrileHCID 6342—
生成物4-Chloro-N-{2-[4-(difluoromethoxy)phenyl]ethyl}-6-methoxy-1,3,5-triazin-2-amineHCID 8961979331.7%

反応手順

A solution of 1.8 g of 2,4-dichloro-6-methoxy-1,3,5-triazine in 40 ml of acetonitrile is cooled on an ice bath, 1.28 ml of DIPEA and then 1.68 g of 2-[4-(difluoromethoxy)phenyl]ethanamine are added and the mixture is stirred for 30 minutes. The reaction mixture is diluted by adding 100 ml of EtOAc and 50 ml of water, the phases are separated by settling, the organic phase is washed with saturated NaCl solution and dried over MgSO4, and the solvent is evaporated off under vacuum. The residue is taken up in DCM, the insoluble matter is filtered off and the filtrate is concentrated under vacuum. The residue is chromatographed on silica gel, eluting with a cyclohexane/EtOAc mixture in a gradient of from (95/5 v/v) to (80/20 v/v). 0.94 g of the expected compound is obtained.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09115121B2
出典データセットuspto-grants-2015_08
ORD IDord-b9beb49da07947d8883b89d17e513bab
出典メモuspto-grants-2015_08