関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl chloroformate | HCID 6586 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | Ethyl 2-cyano-2-(hydroxyimino)acetate | HCID 6399078 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Ethyl 2-methoxycarbonyloxyimino-2-cyanoacetate | HCID 54529457 | 42.2% |
反応手順
A mixture of sodium salt of ethyl 2-hydroxyimino-2-cyanoacetate (16.4 g), water (100 ml) and acetone (15 ml) is stirred at 0°C, and methyl chloroformate (9.4 g) is dropwise added thereto. The resulting mixture is adjusted to pH 7 to 8 with the addition of an aqueous solution of sodium hydrogencarbonate and stirred for 5 hours. The reaction mixture is extracted with ether, and the ether layer is washed with water, dried and concentrated. The residue is recrystallized from a benzene - n-hexane mixture to give ethyl 2-methoxycarbonyloxyimino-2-cyanoacetate (8.4 g) as crystals melting at 69° to 71°C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US03976635 |
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| 出典データセット | uspto-grants-1976_08 |
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| ORD ID | ord-df18ae181235415ca77d12c6e07a5223 |
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| 出典メモ | uspto-grants-1976_08 |
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