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Water → 5-(4-benzyloxycarbonylaminophenyl)-3-methyl-2(1H)-pyrazinone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Pyrazine, 2-chloro-3-methyl- | HCID 66769 | — |
| 反応物 | benzyl N-hydroxy-N-phenylcarbamate | HCID 12358018 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5-(4-benzyloxycarbonylaminophenyl)-3-methyl-2(1H)-pyrazinone | HCID 13853561 | — |
反応手順
To a stirred suspension of sodium hydride (2.1 g, 50% in oil) in dry dimethylformamide (35 ml) with external cooling was added portionwise, benzyl N-hydroxy-N-phenylcarbamate (10.6 g). After 5 minutes a brown solution was obtained to which was added 2-chloro-3-methylpyrazine (5.5 g) and the mixture was allowed to attain room temperature. The solution was poured into water (200 ml) and the aqueous phase decanted from the dark oil. The aqueous solution deposited a yellow solid which was collected and washed with ethanol to give 5-(4-benzyloxycarbonylaminophenyl)-3-methyl-2(1H)-pyrazinone (1.55 g. m.p. 238°-240° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04556711 |
| 出典データセット | uspto-grants-1985_12 |
| ORD ID | ord-b3f42ff6bd44464ba312d37428adc2a6 |
| 出典メモ | uspto-grants-1985_12 |