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Triethylamine → 1-(Isocyanatomethyl)-2,4-dimethoxybenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | P,P-Diphenylphosphinic azide | HCID 199401 | — |
| 反応物 | 2-(2,4-Dimethoxyphenyl)acetic acid | HCID 350555 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-(Isocyanatomethyl)-2,4-dimethoxybenzene | HCID 11252527 | 298.9% |
反応手順
To 2,4-dimethoxyphenylacetic acid (3.92 g, 20 mmol) in dry toluene (100 mL) was added dry triethylamine (2.93 mL, 4.2 mmol) and diphenyl phosphorylazide (4.31 mL, 4 mmol). The mixture was stirred at room temperature for 0.5 hours, and then heated at reflux for a further 3 hours. After cooling, the mixture was concentrated under reduced pressure and purified by distillation using an oil pump to give 2,4-dimethoxybenzyl isocyanate (2.31 g, 60%). IR vmax/cm−1 2243.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08450479B2 |
| 出典データセット | uspto-grants-2013_05 |
| ORD ID | ord-c9186fe9548543bcab9fdbcfa277e52e |
| 出典メモ | uspto-grants-2013_05 |