関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium ethoxide | HCID 2723922 | — |
| 反応物 | Ethyl 2-(4-acetoxy-2-methylphenoxy)acetate | HCID 21986316 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Ethyl (4-hydroxy-2-methylphenoxy)acetate | HCID 21986458 | — |
反応手順
A solution of ethyl[4-(acetyloxy)-2-methylphenoxy]acetate (intermediate 6, 148 g) in ethanol (1300 ml) was treated with sodium ethoxide (41.3 g) and the mixture heated to 45° C. for 2.5 hours. The mixture as cooled to 22° C. and concentrated hydrochloric acid added to give a neutral (pH 7) solution. The resulting mixture was concentrated and the residue dissolved in a mixture of t-butylmethyl ether, water and brine. The organic layer was separated, washed with brine and dried over sodium sulfate and filtered. The filtrate was concentrated to give a brown solid which was further purified by precipitation from a solution in dichloromethane (100 ml) on addition of cyclohexane (710 ml) to give the title compound as a brown solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07091237B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-55f2e447a6be46f59025fb20b44ca092 |
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| 出典メモ | uspto-grants-2006_08 |
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