Phosphonochloridic acid, P-ethenyl-, methyl ester synthesis
- Product Name:Phosphonochloridic acid, P-ethenyl-, methyl ester
- CAS Number:80920-76-9
- Molecular formula:C3H6ClO2P
- Molecular Weight:140.51
4645-32-3
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Yield:80920-76-9 53%
Reaction Conditions:
with oxalyl dichloride in 1,2-dichloro-ethane at 60; for 30 h;Inert atmosphere;
Steps:
Methyl vinylphosphonochloridate (8)
To a solution of dimethyl vinylphosphonate (5, 400 g, 2.94 mol) in 1,2-dichloroethane (2 kg) was added oxalyl chloride (392 g, 3.09 mol) dropwise under nitrogen atmosphere. The resultant mixture was stirred for 30 h at 60 °C. The reaction mixture was cooled to room temperature and concentrated in vacuo. The residue was purified by distillation to give the title compound (220 g, 53 %) as a colorless oil.
References:
Watanabe, Bunta;Morikita, Tatsuya;Tabuchi, Yukiko;Kobayashi, Ryoto;Li, Chunjie;Yamamoto, Masakazu;Koeduka, Takao;Hiratake, Jun [Tetrahedron Letters,2017,vol. 58,# 38,p. 3700 - 3703] Location in patent:supporting information
59268-51-8
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80920-76-9
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