関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Ethyl bromoacetate | HCID 7748 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4,4'-Dichlorobenzophenone oxime | HCID 74389 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Ethyl di-(4-chlorophenyl)methyleneamino-oxyacetate | HCID 12942463 | — |
反応手順
Sodium hydride (0.45 g., 80% w/w suspension in mineral oil) was added gradually to a stirred solution of 4,4'-dichlorobenzophenone oxime (4.0 g.) in dry dimethylformamide (20 ml.) keeping the temperature below 30° C. After 30 minutes, ethyl bromoacetate (1.7 ml.) was added to the stirred solution and the temperature was allowed to rise to 30° C. After 16 hours stirring at ambient temperature the mixture was poured into water (100 ml.) and the subsequent mixture was extracted with ether. The combined extracts were washed with water, dried (MgSO4) and evaporated to give ethyl di-(4-chlorophenyl)methyleneamino-oxyacetate, as an oil (3.8 g.), essentially pure and having a characteristic ester absorption at 1740-1760 cm-1 in the infra-red spectrum.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04176194 |
|---|
| 出典データセット | uspto-grants-1979_11 |
|---|
| ORD ID | ord-0070be7f38a14afa8e5cf102433dffa7 |
|---|
| 出典メモ | uspto-grants-1979_11 |
|---|