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Phosgene → 5-Isocyanato-1,2,3-trimethoxybenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosgene | HCID 6371 | — |
| 反応物 | 3,4,5-Trimethoxyaniline | HCID 32285 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 5-Isocyanato-1,2,3-trimethoxybenzene | HCID 517766 | — |
反応手順
A mixture of 3,4,5-trimethoxyaniline (365 mg; 2.0 mmol) in toluene (20 ml) and phosgene (6 ml 20% in toluene; 12 mmol) was refluxed for 6 h. The solvent was removed under reduced pressure to give crude 3,4,5-trimethoxyphenylisocyanate. The crude product was added 3-[4-(4-chloro-phenyl)-1-piperazinyl]propanol (800 mg; 3.1 mmol) in toluene (25 ml) and refluxed for 16 h. The solvent was evaporated and the residue taken up in ethanol, which was treated with hydrogen chloride in ether. Recrystallization from ethanol/ether afforded 620 mg of the title compound M.p. 173.5°-174.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05246935 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-c66e87f2688c4345b675a14629eb0241 |
| 出典メモ | uspto-grants-1993_09 |