関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylamine | HCID 674 | — |
| 反応物 | Hexamethylphosphorous triamide | HCID 15355 | — |
| 反応物 | 1,4,8-Triazacycloundecane | HCID 398742 | — |
| 生成物 | Hexahydro-2a,5a,8a-triaza-8b-phospha-acenaphthylene | HCID 23414755 | 75.2% |
反応手順
A mixture of 3.62 g of 1,4,8-triazacycloundecane and 3.75 g of hexamethylphosphorous triamide is heated to 125° C with stirring and held at this temperature for 2 hours, by which time evolution of dimethylamine is complete. Evolution is vigorous for the first 45 minutes. Distillation affords 3.20 g (75%) 1,4,8-triaza-12-phosphatricyclo-[6.3.1.04,12 ]dodecane as a water-white liquid which boils at 73°-75° C at 0.30 mm.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US03996276 |
|---|
| 出典データセット | uspto-grants-1976_12 |
|---|
| ORD ID | ord-b13e99e974744e3a9603d095231b7332 |
|---|
| 出典メモ | uspto-grants-1976_12 |
|---|
