関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodoethane | HCID 6340 | — |
| 反応物 | Carbon Disulfide | HCID 6348 | — |
| 反応物 | Chloroacetone | HCID 6571 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 3-Oxobutyronitrile | HCID 75579 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 20068980 | HCID 20068980 | — |
反応手順
To a suspension of 10.5 g of sodium salt of cyanoacetone in 200 ml of dimethylformamide 9.0 ml of carbon disulphide are gradually added while stirring cooling in ice and keeping under nitrogen, succeeded by 4.5 g of sodium hydride dispersion. After stirring for an hour with cooling, 8.4 ml of chloroacetone are added dropwise under the same reaction conditions. After stirring for another hour, 0.4 g of powdered NaOH are added and finally, after again stirring for another 0.5 hour, 8.0 ml of ethyl iodide under the same conditions. After stirring, the reaction mixture for again another hour and leaving to stand overnight it is poured 1 l of ice water and extracted with diethyl ether. The organic phase is washed with water three times, dried, treated with charcoal, filtered and evaporated. After recrystallisation from isopropanol, the residue yields the desired product in a yield of 9.54 g; melting-point 51°-52° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04994485 |
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| 出典データセット | uspto-grants-1991_02 |
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| ORD ID | ord-5ca4d5a75a124d0a8296a3c6089d58fd |
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| 出典メモ | uspto-grants-1991_02 |
|---|