関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Urea | HCID 1176 | — |
| 反応物 | Ephedrine | HCID 9294 | — |
| 反応物 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 反応物 | Ammonium sulfamate | HCID 24482 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1,5-Dimethyl-4-phenylimidazolidin-2-one | HCID 230547 | — |
反応手順
1 mol of an ephedrine, 1.025 mol of ammonium sulfamate, 3 mol of urea and the proton-donating compound were introduced into 200 ml of NMP. The reaction mixture was heated to 175 to 180° C. and stirred at this temperature for 2.5 h. It was then cooled to 130° C. and, at this temperature, water was added dropwise to the reaction mixture. Two phases formed. The lower phase was removed at 95° C. The upper phase was further cooled initially to 65° C. Crystals formed at this temperature. It was cooled further to 10° C. and stirred at this temperature for 1 h. The crystals were filtered off with suction and washed twice with cold water. The solid was dried in vacuo at RT overnight.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07365210B2 |
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| 出典データセット | uspto-grants-2008_04 |
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| ORD ID | ord-0c674f87262c463884a0803402d2a8e9 |
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| 出典メモ | uspto-grants-2008_04 |
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