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

HRID 921346

반응식

HRID 921346 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 668332461-Benzyl-4-methyl-1,4-azaphosphinane 4-oxide수율 70.3%

시약·촉매·용매 1

HCID 21881883Oxolane--water (1/1)용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-6741e95f9a5142949dd146190e550bbb
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09273077B2

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