Azobisisobutyronitrile → HCID 11762403、化合物

反応式

[PH:1]([CH2:4][CH3:5])[CH2:2][CH3:3].N([C:13]([CH3:17])([CH3:16])C#N)=NC(C)(C)C#N>>[CH2:17]([P:1]([CH2:4][CH2:5][P:1]([CH2:4][CH3:5])[CH2:2][CH3:3])[CH2:2][CH2:3][P:1]([CH2:4][CH3:5])[CH2:2][CH3:3])[CH2:13][CH3:16]

参加物

反応物 2

HCID 6547Azobisisobutyronitrile

HCID 82948Phosphine, diethyl-

生成物 1

HCID 11762403HCID 11762403、化合物収率 5,502.7%

実験手順

A mixture of n-PrP(CH=CH2)2 (1.29 g, 10.0 mmol), Et2PH (2.25 g, 25.0 mmol) and 2,2'-azobis(isobutyronitrile) (AIBN, 30 mg) in a closed flask under inert atmosphere was irradiated by a GE Sunlamp (275 W) one foot away for 24 hours. The resulting colorless liquid was stripped of volatiles under vacuum and vacuum distilled to give 3.1 g (97% yield) of product collected at 132-135° C./0.35 mm Hg. 31P-NMR (toluene): δ--18.5 (2P); δ--22.8 (1P).

後処理

customwas irradiated by a GE Sunlamp (275 W) one foot away for 24 hours
distillationdistilled

出典と根拠

ORDレコード: ord-3613d0adbe0249cead14e1366770dabb
出典データセット: uspto-grants-1999_10
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US05968866

反応ノート

読み込み中…

参加物