化工社化工社 化学情報印刷レポート · 研究参考用
Phosphorus trichloride → Diisopropylphosphoramidous dichloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphorus trichloride | HCID 24387 | — |
| 反応物 | Bis(diisopropylamino)chlorophosphine | HCID 2733425 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Diisopropylphosphoramidous dichloride | HCID 5139911 | 81% |
反応手順
Bis-(N,N-Diisopropylamino) chlorophosphine, 10 grams (37 mmols), was dissolved in 500 ml of anhydrous acetonitrile. Phosphorus trichloride, 5.16 grams (37 mmols), was added to the solution and the reaction was allowed to stir over-night at room temperature. The reaction was assayed for completion by 31P NMR of an aliquot of the reaction using an external lock. Complete conversion of the starting material at δ 134 ppm to the product at δ 165 ppm was observed. The solvent was evaporated from the reaction mixture on a rotary evaporator and the resulting oil distilled under vacuum yielding 5.7 grams of product (81% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07745591B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-0360ccbca2fd4ed99002b89ee7ec54f8 |
| 出典メモ | uspto-grants-2010_06 |