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N,N-Dimethylaniline → 2,6-Di(propan-2-yl)phenyl carbonochloridate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N,N-Dimethylaniline | HCID 949 | — |
| 反応物 | Propofol | HCID 4943 | — |
| 反応物 | Phosgene | HCID 6371 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2,6-Di(propan-2-yl)phenyl carbonochloridate | HCID 271619 | — |
反応手順
To a cooled (0° C.) solution of propofol (20.0 g, 112 mmol) in toluene (40 mL) was added phosgene (82 mL, 20% in toluene) under a nitrogen atmosphere. The reaction mixture was stirred for 5 min, and then N,N-dimethylaniline (15 mL, 118 mmol) was added dropwise. The mixture was allowed to warm to room temperature slowly and stirred for 14 h. The suspended mixture was then filtered. The filtrate was collected and the solvent was removed in vacuo. The remaining crude product (9) was carried to the next step without further purification. 1H-NMR (400 MHz, CDCl3): δ 7.18-7.29 (m, 3H), 3.00-3.07 (m, 2H), 1.25-1.27 (d, J=6.8 Hz, 12H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08067455B2 |
| 出典データセット | uspto-grants-2011_11 |
| ORD ID | ord-d02b3c3fdfdd4b3691ca89641b90487c |
| 出典メモ | uspto-grants-2011_11 |