Acetoxyacetyl chloride → 2-{[3-Acetyl-6-(4-chlorophenyl)-7-(2,4-dichlorophenyl)-1-methyl-2-oxo-1,2-dihydro-1,8-naphthyridin-4-yl]amino}-2-oxoethyl acetate

関与物質

役割	名称	HCID	仕込み量
反応物	Acetoxyacetyl chloride	HCID 26297	—
反応物	3-acetyl-4-amino-6-(4-chlorophenyl)-7-(2,4-dichlorophenyl)-1-methyl-1,8-naphthyridin-2(1H)-one	HCID 11260007	—
溶媒	Acetonitrile	HCID 6342	—
溶媒	Ethyl Acetate	HCID 8857	—
生成物	2-{[3-Acetyl-6-(4-chlorophenyl)-7-(2,4-dichlorophenyl)-1-methyl-2-oxo-1,2-dihydro-1,8-naphthyridin-4-yl]amino}-2-oxoethyl acetate	HCID 11365162	—

反応条件

温度	90 °C

反応手順

To the product of Example 2 (120 mg) in acetonitrile (2 mL) was added acetoxyacetyl chloride (0.2 mL). The reaction was heated to 90° C. in a CEM microwave reactor for a total of 34 minutes. The reaction was diluted with EtOAc and was washed with saturated aqueous NaHCO3 solution. The concentrated residue was purified by flash chromatography on silica gel gradient eluted with 0-60% EtOAc in hexane affording the title compound. HPLC/MS: 572.1 (M+1), 574.1 (M+3); Rt=4.06 min.

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US07728141B2
出典データセット	uspto-grants-2010_06
ORD ID	ord-6bbe050a73ec42f596a556812d626ba7
出典メモ	uspto-grants-2010_06