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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 | Dimethylhydantoin | HCID 6491 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 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 1,458 ml of dimethylformamide is reacted for 18 hours and 20 minutes at 90° C to 100° C internal temperature (external temperature 155° C), whilst constantly removing the resulting water of reaction by azeotropic circulatory distillation. Water of reaction eliminated: 110 g (94.0% of theory). Thereafter the reaction mixture, whilst still hot, is separated by filtration from the potassium chloride produced, the filtrate concentrated on a rotary evaporator at 100° C 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 | US03994858 |
| 出典データセット | uspto-grants-1976_11 |
| ORD ID | ord-7521e075204e4d1b9be21e562ff7b6d9 |
| 出典メモ | uspto-grants-1976_11 |