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Water → 2-(5-Tert-butyl-2-hydroxy-4-nitrophenyl)-2-methylpropanoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-(1-Amino-2-methyl-1-oxopropan-2-yl)-4-tert-butyl-5-nitrophenyl methyl carbonate | HCID 59544163 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-(5-Tert-butyl-2-hydroxy-4-nitrophenyl)-2-methylpropanoic acid | HCID 59544150 | — |
反応手順
To a mixture of compound 17 (7.3 g, 21.6 mmol) in methanol (180 mL) was added water (18 mL) and NaOH (8.64 g, 216 mmol). The solution was heated and maintained at reflux for 3 days. The solvent was evaporated in vacuo and the residue was dissolved in 140 mL of water. Then the solution was acidified to pH 2 by the addition of 2N HCl. The aqueous phase was extracted with ethyl acetate (100 mL×3), and the combined organic phases were washed with water and brine, dried over anhydrous Na2SO4 and then concentrated to give compound 18 as a yellow solid, which was used in the next reaction without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08835639B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-4427781082e3430b827ae41f560b31e3 |
| 出典メモ | uspto-grants-2014_09 |