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Methyl chloroformate → Ethyl 2-methoxycarbonyloxyimino-2-cyanoacetate
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 | 82.2% |
反応手順
A solution of sodium salt of ethyl 2-hydroxyimino-2-cyanoacetate (41.0 g) in water (200 ml) is stirred under ice-cooling, and a solution of methyl chloroformate (23.6 g) in acetone (20 ml) is dropwise added thereto. The resulting mixture is adjusted to pH 6 to 7 with the addition of an aqueous solution of sodium hydrogencarbonate and stirred for 1 hour. The precipitates are collected by filtration, washed with water and dried to give ethyl 2-methoxycarbonyloxyimino-2-cyanoacetate (41.1 g) as crystals melting at 68° to 70°C which is identified with the compound obtained in Example 9 by IR absorption spectrum.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US03976635 |
| 出典データセット | uspto-grants-1976_08 |
| ORD ID | ord-a6efa27fada64675bfa5c09f9ee5470a |
| 出典メモ | uspto-grants-1976_08 |