関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 反応物 | 1-(2-Ethyl-butyl)-cyclohexanecarboxylic acid ethyl ester | HCID 44548657 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-(2-Ethyl-butyl)-cyclohexanecarboxylic acid | HCID 10488751 | 99% |
反応手順
1-(2-Ethyl-butyl)-cyclohexanecarboxylic acid ethyl ester (2.0 g, 8.32 mmol) was added dropwise under stirring to a solution of KOtBu (3.735 g, 33.3 mmol) in THF (15 mL) containing a small amount of water (225 mg, 12.5 mmol). The mixture was stirred 20 h at 54° C., cooled to room temperature, slowly poured onto a mixture of ice and 4N H2SO4 and extracted with DCM (2×150 mL) after adjusting to pH 1. The organic phases were washed with diluted aq. NaCl (100 mL), combined, dried over sodium sulfate and concentrated to afford 1.748 g (99%) 1-(2-ethyl-butyl)-cyclohexanecarboxylic acid, purity 95.2% (GC with internal standard).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08071803B2 |
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| 出典データセット | uspto-grants-2011_12 |
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| ORD ID | ord-e3e70bedcb2a4ab894ae78d447ed972d |
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| 出典メモ | uspto-grants-2011_12 |
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