反応式
C(N([P:8]([N:10]([CH:14]([CH3:16])[CH3:15])[CH:11]([CH3:13])[CH3:12])[Cl:9])C(C)C)(C)C.P(Cl)(Cl)[Cl:18]>C(#N)C>[CH:11]([N:10]([P:8]([Cl:18])[Cl:9])[CH:14]([CH3:16])[CH3:15])([CH3:13])[CH3:12]参加物
4
実験手順
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).
後処理
- customThe solvent was evaporated from the reaction mixture on a rotary evaporator
- distillationthe resulting oil distilled under vacuum
出典と根拠
- ORDレコード
- ord-0360ccbca2fd4ed99002b89ee7ec54f8
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07745591B2
関連ノート
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