関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 4-Chlorobenzene-1-carboximidamide hydrochloride | HCID 203436 | — |
| 反応物 | Diethyl 2-oxosuccinate,sodium salt | HCID 57351814 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(4-Chlorophenyl)-6-hydroxypyrimidine-4-carboxylic acid | HCID 135878882 | 45% |
反応手順
To a mixture of diethyl oxalacetate sodium salt (123.2 g, 586 mmol) in water (750 mL) was slowly added aqueous sodium hydroxide (50%, 47 g, 586 mmol). After 1 h the solids had dissolved. 4-Chlorobenzenecarboximidamide monohydrochloride (111.95 g, 586 mmol) was then added, and the mixture was heated at 70° C. overnight. After cooling to room temperature concentrated hydrochloric acid was slowly added (causing foaming) until the pH was lowered to 1.5. The solid was isolated by filtration and washed with water and methanol. The solid was then triturated twice with hot methanol, washed repeatedly with 1 N hydrochloric acid, then once with methanol and dried to afford the title compound (66.07 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07863220B2 |
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| 出典データセット | uspto-grants-2011_01 |
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| ORD ID | ord-8e1ddbf19327444aa4e98e53193ac2aa |
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| 出典メモ | uspto-grants-2011_01 |
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