Benzylamine → 1-Benzyl-4-methyl-1,4-azaphosphinane 4-oxide

HRID 921414ノート

反応式

HRID 921414 の反応式
[CH3:1][P:2](=[O:7])([CH:5]=[CH2:6])[CH:3]=[CH2:4].[CH2:8]([NH2:15])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1>C1COCC1.O>[CH2:8]([N:15]1[CH2:6][CH2:5][P:2](=[O:7])([CH3:1])[CH2:3][CH2:4]1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

参加物

4

反応物 2

HCID 7504BenzylamineHCID 57973285(Ethenyl(methyl)phosphoryl)ethene

生成物 1

HCID 668332461-Benzyl-4-methyl-1,4-azaphosphinane 4-oxide収率 70.3%

試薬・触媒・溶媒 1

HCID 21881883Oxolane--water (1/1)溶媒

実験手順

A solution of methyl divinyl phosphine oxide (1.16 g, 10.0 mmol) and benzylamine (1.20 mL, 11.0 mmol) in 1:1 THF/water (25 mL) was heated at reflux for 16 h. The reaction mixture was concentrated in vacuo and the residue was purified by silica gel chromatography (0-10% 7N ammonia in methanol:dichloromethane) to afford 1-benzyl-4-methyl-[1,4]azaphosphinane-4-oxide as a white solid (1.57 g, 70% yield).

後処理

  1. temperatureat reflux for 16 h
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. customthe residue was purified by silica gel chromatography (0-10% 7N ammonia in methanol:dichloromethane)

出典と根拠

ORDレコード
ord-139d0d9ddcea4e31963458b0f2a6cc9c
出典データセット
uspto-grants-2016_03
特許番号
US09273077B2

反応ノート

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