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HRID 1682720作成日:2026年10月25日

Benzene → 2-[2-(4-Methoxycarbonylmethylphenoxy)-1-methylethyl]amino-1-(3,5-di-t-butyl-4-hydroxyphenyl)ethanol

https://huagongshe.com/reaction/1682720

反応式

関与物質

役割名称HCID仕込み量
反応物BenzeneHCID 241—
反応物Sodium cyanoborohydrideHCID 5003444—
反応物2-Amino-1-(3,5-di-t-butyl-4-hydroxyphenyl)ethanolHCID 21832163—
反応物Methyl 4-(2-oxopropoxy)phenylacetateHCID 21832178—
溶媒MethanolHCID 887—
生成物2-[2-(4-Methoxycarbonylmethylphenoxy)-1-methylethyl]amino-1-(3,5-di-t-butyl-4-hydroxyphenyl)ethanolHCID 2183218945%

反応手順

A procedure similar to that described in Example 6 was repeated, except that 3 g of 2-amino-1-(3,5-di-t-butyl-4-hydroxyphenyl)ethanol (prepared as described in Preparation 35), 2.2 g of methyl 4-(2-oxopropoxy)phenylacetate (prepared as described in Preparation 3), 100 ml of benzene, 60 ml of absolute methanol and 4 g of sodium cyanoborohydride were used, and that the product was purified by repeated column chromatography through silica gel, using as the eluent first ethyl acetate and then a 1:1 by volume mixture of benzene and ethyl acetate. 2.1 g of 2-[2-(4-methoxycarbonylmethylphenoxy)-1-methylethyl]amino-1-(3,5-di-t-butyl-4hydroxyphenyl)ethanol were obtained. This product was then mixed with 246 mg of fumaric acid, and the mixture was recrystallized from ethyl acetate, to give 1.5 g of the title compound as crystals, melting at 171°-174° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05635534
出典データセットuspto-grants-1997_06
ORD IDord-c0434956589f4b19b1168fc9a9f73fd9
出典メモuspto-grants-1997_06