関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Lithium hydroxide, monohydrate | HCID 168937 | — |
| 反応物 | Ethyl 4-((tert-butyldimethylsilyl)oxy)cyclohexanecarboxylate | HCID 23144129 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-[[(1,1-Dimethylethyl)dimethylsilyl]oxy]cyclohexanecarboxylic acid | HCID 57960710 | 75.7% |
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
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08637546B2 |
|---|
| 出典データセット | uspto-grants-2014_01 |
|---|
| ORD ID | ord-d2116a79fad84b12ab887829a645660d |
|---|
| 出典メモ | uspto-grants-2014_01 |
|---|