関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Sodium Azide | HCID 33557 | — |
| 反応物 | 1-Naphthalenecarboxamide | HCID 75244 | — |
| 生成物 | HCID 178522022 | HCID 178522022 | 84% |
反応手順
The above naphthoic acid amide (10 g, 37 mmol) was dissolved in N,N-dimethylformamide (200 mL) and sodium azide (2.63 g, 40 mmol) and ammonium chloride (2.16 g, 40 mmol) were added and the mixture heated at 125° C. for 6 hours. Sodium azide (1.2 g) and ammonium chloride (0.98 g) were added and the mixture heated at 125° C. for 16 hours. After cooling, the mixture was poured into water (1.5 l) and stirred at room temperature for 30 minutes. The solid formed was filtered off, washed with water and dried in vacuo at 50° C. for 3 days affording 9.69 g (84%) of the title compound as a solid which could be further purified by treatment with ethanol at reflux temperature.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07879893B2 |
|---|
| 出典データセット | uspto-grants-2011_02 |
|---|
| ORD ID | ord-ad7e8a19ac1b4ecbaef897dc545dbbd1 |
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| 出典メモ | uspto-grants-2011_02 |
|---|