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HRID 475377作成日:2026年10月25日

Lithium hydroxide, monohydrate → 4-[[(1,1-Dimethylethyl)dimethylsilyl]oxy]cyclohexanecarboxylic acid

https://huagongshe.com/reaction/475377

反応式

関与物質

役割名称HCID仕込み量
反応物Lithium hydroxide, monohydrateHCID 168937—
反応物Ethyl 4-((tert-butyldimethylsilyl)oxy)cyclohexanecarboxylateHCID 23144129—
溶媒MethanolHCID 887—
溶媒TetrahydrofuranHCID 8028—
生成物4-[[(1,1-Dimethylethyl)dimethylsilyl]oxy]cyclohexanecarboxylic acidHCID 5796071075.7%

反応条件

温度60 °C

反応手順

To a solution of Example 45A (6.6 g, 23.0 mmol) in tetrahydrofuran (31 mL) and methanol (20 mL) was added lithium hydroxide monohydrate (1.93 g, 46.1 mmol). The resulting mixture was heated at 60° C. for 2 hours. The heat was removed and the reaction mixture was stirred at room temperature overnight. The solvents were removed in vacuo and the solution was neutralized with 1M HCl. Ethyl acetate (200 mL) was added and the layers were separated. The aqueous layer was further extracted with ethyl acetate (2×200 mL). The combined organic layers were dried over sodium sulfate, filtered and concentrated to give the titled compound (4.5 g). MS (CI) m/z 259 (M+1)+

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08637546B2
出典データセットuspto-grants-2014_01
ORD IDord-d2116a79fad84b12ab887829a645660d
出典メモuspto-grants-2014_01