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1,2-Dichloroethane → 3-(2-Chloroethyl)-5,5-dimethylimidazolidine-2,4-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Dimethylhydantoin | HCID 6491 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-(2-Chloroethyl)-5,5-dimethylimidazolidine-2,4-dione | HCID 298085 | — |
反応手順
A mixture of 1,664 g of 5,5-dimethyl-hydantoin (13.0 mols), 897 g of anhydrous potassium carbonate (6.5 mols), 5,148 g of 1,2-dichloroethane (52 mols) and 1,485 ml of dimethylformamide is reacted for 18 hours and 20 minutes at 90°C to 100°C internal temperature (external temperature 155°C), the water of reaction produced being removed continuously by azeotropic circulatory distillation. Water of reaction split off: 110 g (94.0% of theory). Thereafter, the reaction mixture, whilst still hot, is separated by filtration from the potassium chloride produced, the filtrate is concentrated on a rotary evaporator at 100°C in a water pump vacuum and the residue is dried to constant weight at 100°C and 10-1 mm Hg.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US03978076 |
| 出典データセット | uspto-grants-1976_08 |
| ORD ID | ord-14960d29a99447eab6747798a10f6906 |
| 出典メモ | uspto-grants-1976_08 |