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Carbon Disulfide → 1,2-Bis(4-diethylamino-2-methylphenyl)ethane-1,2-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Carbon Disulfide | HCID 6348 | — |
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 反応物 | N,N-diethyl-m-toluidine | HCID 66679 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 1,2-Bis(4-diethylamino-2-methylphenyl)ethane-1,2-dione | HCID 13782103 | 23.3% |
反応手順
To 8.3 g of anhydrous aluminum chloride, 30 ml of carbon disulfide was added, followed by dropwise addition of 16.3 g of N,N-diethyl-m-toluidine under ice-cooling. Then, 5 g of oxalyl chloride was added dropwise thereto at 5° C. or lower, and reacted for 1 hour with stirring. After the reaction, 50 ml of water and 100 ml of chloroform were added to the reaction solution. The chloroform layer obtained by separation was washed with 2N hydrochloric acid, dried and concentrated. The residue was recrystallized from ethyl acetate to yield 3.5 g of yellow 1,2-bis(4-diethylamino-2-methylphenyl)ethane-1,2-dione.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05164512 |
| 出典データセット | uspto-grants-1992_11 |
| ORD ID | ord-f940ba0a035943f89c458d4521051fe5 |
| 出典メモ | uspto-grants-1992_11 |