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HRID 337587作成日:2026年10月26日

Dichloromethane → 2-[3,4-Dichloro-5-({[(1,1-dimethylethyl)(dimethyl)silyl]oxy}methyl)phenyl]ethyl methanesulfonate

https://huagongshe.com/reaction/337587

反応式

関与物質

役割名称HCID仕込み量
反応物DichloromethaneHCID 6344—
反応物Methanesulfonyl chlorideHCID 31297—
反応物DiisopropylethylamineHCID 81531—
反応物2-[3,4-Dichloro-5-({[(1,1-dimethylethyl)(dimethyl)silyl]oxy}methyl)phenyl]ethanolHCID 66895403—
溶媒Diethyl EtherHCID 3283—
生成物2-[3,4-Dichloro-5-({[(1,1-dimethylethyl)(dimethyl)silyl]oxy}methyl)phenyl]ethyl methanesulfonateHCID 86651668—

反応条件

温度0 °C

反応手順

To a dichloromethane (0.11 M) solution of 2-[3,4-dichloro-5-({[(1,1-dimethylethyl)(dimethyl)silyl]oxy}methyl)phenyl]ethanol (1 eq.) from the previous step was added at 0° C. Hunig's base (1.5 eq.) and methanesulfonyl chloride (1.1 eq.). The resulting suspension was stirred at 0° C. for 30 min and at RT for 15 min. The reaction was then diluted with ether and quenched with 1N aq. HCl. The aqueous layer was separated and back-extracted with ether. The combined organic extracts were washed further with 1 N aq. NaOH, water and brine, dried over Na2SO4, filtered and the filtrate concentrated in vacuo to give the title compound as a brown oil.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08889714B2
出典データセットuspto-grants-2014_11
ORD IDord-ba30d19d5c82457cabbcda5757a1e3a4
出典メモuspto-grants-2014_11