1-Hydroxybenzotriazole → Methyl 3-[2-({[4-(3,4-dichlorobenzyl)morpholin-2-yl]methyl}amino)-2-oxoethyl]benzoate

関与物質

役割	名称	HCID	仕込み量
反応物	1-Hydroxybenzotriazole	HCID 75771	—
反応物	Diisopropylethylamine	HCID 81531	—
反応物	1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride	HCID 2723939	—
反応物	2-(3-(methoxycarbonyl)phenyl)acetic acid	HCID 13816152	—
反応物	1-[4-[(5-Chlorothien-2-yl)methyl]morpholin-2-yl]methanamine	HCID 21962888	—
溶媒	Dichloromethane	HCID 6344	—
生成物	Methyl 3-[2-({[4-(3,4-dichlorobenzyl)morpholin-2-yl]methyl}amino)-2-oxoethyl]benzoate	HCID 21963019	57.2%

反応条件

温度	20 °C

反応手順

A mixture of [3-(methoxycarbonyl)phenyl]acetic acid (0.200 g), Intermediate 1 (0.284 g), 1-hydroxybenzotriazole (0.182 g) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (0.316 g) was stirred in dichloromethane (10 ml), and N,N-diisopropylethylamine (0.352 ml) was added to the solution. Stirring at 20° C. under nitrogen was continued for 8 h. The mixture was purified by solid phase extraction (2×10 g Varian Bondelut silica gel cartridges), eluting successively with one column volume of dichloromethane, chloroform, ether, ethyl acetate, acetone, acetonitrile and methanol, to give the title compound as a colourless gum, (0.266 g).

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US07560548B2
出典データセット	uspto-grants-2009_07
ORD ID	ord-9e76dd28952e4fc99ac98cab9379cab8
出典メモ	uspto-grants-2009_07