Carbonic acid--N,N-diethylethanamine (1/2) → 4-Phenyl-1,4lambda5-azaphosphinan-4-one

HRID 562440Notes

Reaction equation

HRID 562440 reaction equation
Cl.[C:2]1([P:8]2(=[O:14])[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CC[NH+](CC)CC.CC[NH+](CC)CC.C([O-])([O-])=O>O>[C:2]1([P:8]2(=[O:14])[CH2:9][CH2:10][NH:11][CH2:12][CH2:13]2)[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Participants

4

Reactant 2

HCID 15264167Carbonic acid--N,N-diethylethanamine (1/2)HCID 668324724-Phenyl-1,4lambda5-azaphosphinan-4-one hydrochloride

Product 1

HCID 579259574-Phenyl-1,4lambda5-azaphosphinan-4-one

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

To a 500 mL round-bottom flask was added 4-phenyl-[1,4]azaphosphinane 4-oxide hydrochloride salt (5.91 g, 25.6 mmole), MP-carbonate resin (20 g, 2.9 mmole/g), and water (200 mL). The flask was sealed with a plastic stopper and placed on an orbital shaker for 12 hours. The resin was then removed by filtration with though a glass frit, and washed with water (40 mL) to provide 4-phenyl-[1,4]azaphosphinane 4-oxide free-base as an aqueous solution.

Workup

  1. customThe flask was sealed with a plastic stopper
  2. customThe resin was then removed by filtration with though a glass frit
  3. washwashed with water (40 mL)

Sources & evidence

ORD record
ord-1bf703f176954a74ba3d3cd4fb124ac3
Source dataset
uspto-grants-2011_11
Patent number
US08067395B2

Reaction notes

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