DIETHYL VINYLPHOSPHONATE synthesis
- Product Name:DIETHYL VINYLPHOSPHONATE
- CAS Number:682-30-4
- Molecular formula:C6H13O3P
- Molecular Weight:164.14
5324-30-1
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682-30-4
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Yield:682-30-4 90%
Reaction Conditions:
with potassium hydroxide in ethanolReflux;
Steps:
3.ii
A 150 ml two-necked round bottom flask was filled with EtOH (85 ml). KOH pellets (2.52 g, 0.045 mol) were added. The mixture was stirred in an ice bath until complete KOH dissolution. Diethyl (2-bromoethyl)phosphonate (1) (8.1 ml, 0.045 mol) was added dropwise (30 minutes) by means of an equalizing pressure funnel. Meanwhile a white solid formed. The mixture was refluxed for 15 minutes, and, after cooling, was filtered using a frit. The white solid was washed with absolute EtOH and the filtrate was roto-evaporated, and finally dried under a vacuum pump for 15 minutes. The residue was distilled with a micro-distillator. The first fraction (43° C., 0.5 mmHg) corresponded to pure diethyl vinylphosphonate (3) (yield 90%).1H NMR (CDCl3): δ(ppm)=5.99-6.36 (3H), 4.09 (m, 4H), 1.33 (t, 6H).31P{1H} (CDCl3): δ(ppm)=18.1.
References:
NIHON MED-PHYSICS CO., LTD. US2010/160615, 2010, A1 Location in patent:Page/Page column 11-12
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682-30-4
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80436-45-9
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682-30-4
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