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HRID 56291作成日:2026年10月25日

Toluene → HCID 90023125、化合物

https://huagongshe.com/reaction/56291

反応式

関与物質

役割名称HCID仕込み量
反応物TolueneHCID 1140—
反応物Ammonium ChlorideHCID 25517—
反応物2-(4-Chloronaphthalen-1-yl)oxyacetamideHCID 302908—
反応物N-(3-chloro-4-morpholinophenyl)-3-oxobutanamideHCID 90022603—
触媒Titanium isopropoxideHCID 11026—
溶媒O-XyleneHCID 7237—
生成物HCID 90023125HCID 9002312556.4%

反応条件

温度165 °C

反応手順

A mixture of N-(3-chloro-4-morpholinophenyl)-3-oxobutanamide (0.59 g, 2.0 mmol), 2-((4-chloronaphthalen-1-yl)oxy)acetamide (0.94 g, 4.0 mmol) and titanium tetraisopropanolate (4.8 mL) in xylene (10 mL) was stirred at 165° C. for 24 h. The mixture was cooled to rt and 60 mL of toluene and 60 mL of saturated NH4Cl aqueous solution were added. The resulting mixture was stirred at rt overnight and filtered and the filtrate was extracted with DCM (20 mL×4). The combined organic layers were washed with brine (30 mL×2), dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=1:1) to give the title compound as a yellow solid (0.56 g, 56%). The compound was characterized by the following spectroscopic data:

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09434695B2
出典データセットuspto-grants-2016_09
ORD IDord-4cc9c14f70554901a9650347b7165ece
出典メモuspto-grants-2016_09