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O-Cresol → 1,3-Dimethyl-5-(methoxycarbonyl-methylene)-hydantoin
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | O-Cresol | HCID 335 | — |
| 反応物 | N,N'-Dimethylurea | HCID 7293 | — |
| 反応物 | Dimethylmaleate | HCID 5459894 | — |
| 溶媒 | 1,2-Dichlorobenzene | HCID 7239 | — |
| 生成物 | 1,3-Dimethyl-5-(methoxycarbonyl-methylene)-hydantoin | HCID 54096441 | — |
反応手順
44 g of N,N'-dimethylurea were dissolved in 150 g of o-dichlorobenzene and reacted with 72 g of dimethylmaleate for 2 hours at 180°-185° C after the addition of 25 g of cresol. The solvent was removed from this reaction mixture and the residue was fractionated under vacuum, 85 g (= 85% of the theory) of the desired product distilling over at 0.07 Torr and 128° C. A purified product melting at 49.5° C could be obtained by dissolving the crude product in chloroform and reprecipitating it with ether. The structure of the purified product was confirmed by IR and NMR spectra and by elementary analysis.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04089860 |
| 出典データセット | uspto-grants-1978_05 |
| ORD ID | ord-57af96b92cdb484db5e792ce9ad2d545 |
| 出典メモ | uspto-grants-1978_05 |