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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
A 20% solution of phosgene in toluene (139 mL, 0.269 mol) was added to a stirring solution of propofol (40 g, 0.225 mmol) in toluene (80.0 mL) under a nitrogen atmosphere at 0° C. N,N-Dimethylaniline (34.0 mL, 0.269 mmol) was added dropwise over 15 minutes. The reaction mixture was allowed to warm to room temperature slowly and stirred for 14 h. The reaction mixture was filtered through Celite and the solvent was removed in vacuo. The crude product (2) was carried to the next step without further purification. 1H-NMR (400 MHz, CDCl3): δ 7.29-7.25 (m, 1H), 7.19-7.17 (m, 2H), 3.04-3.01 (m, 2H), 1.25 (d, J=7.2 Hz, 12H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07241807B2 |
| 出典データセット | uspto-grants-2007_07 |
| ORD ID | ord-c0c53cf3640244a9a79b79609bb36484 |
| 出典メモ | uspto-grants-2007_07 |