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Preparation of High Quality Ethephon Using Domestic Diester bis-(2-chloroethyl)-2-chloroethylphosphonate as Substrate
Asian Journal of Chemistry,
Vol. 25 No. 11 (2013): Vol 25 Issue 11
Abstract
Ethephon has been widely used globally. However, few companies can manufacture high quality ethephon with content of 90% in China mainland. This work described a practical procedure, which utilizing bis-(2-chloroethyl)-2-chloroethylphosphonate 2 produced by local Chinese companies as substrate to prepare ethephon with content of over 90 % and high yield.
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- H.M. Zhang, Shanxi Sci. Technol., 6, 53 (2001).
- S. Gerhard, R. Karl and S. Otto, Process for the Manufacture of 2-Chloroethane-Phosphonic acid: GB patent, 1373513 (1974).
- D.I. Randall and C. Vogel, Preparation of 2-Haloethylphosphonic Acid: US Patent, 3808265 (1974).
- D.I. Randall and R.W. Wynn, Mono-2-haloethyl Esters of 2-Haloethanephosphonic Acid: US Patent, 3626037 (1971).
- J.E. Drach and B.J. Pendell, Process for the Manufacture of Aliphatic Phosphonic Acids: US Patent, 4064163 (1977).
- K.W. Young and J.J. Zullo, Process for the Production of Aliphatic Phosphonic Acid: US Patent, 4728466 (1988).
- L. Cauret, J.C. Brosse, D. Derouet and H. De Livonnière, Synth. Commun., 27, 647 (1997).
- L.R. An, C.H. Wang and M.Q. Li, Jiangsu Agrochemicals, 4, 21 (1998).
- GC internal standard method to measure content of ethephon: The ethephon was firstly converted completely into methyl ester by diazonium methane to give dimethyl 2-chloroethyl phosphonate (5), which content can be determined by GC through 10%SE-30 / Gas Chrom Q chromatography using p-nitrochlorobenzene as internal standard solution Through this way, the content of ethephon could be measured.
References
H.M. Zhang, Shanxi Sci. Technol., 6, 53 (2001).
S. Gerhard, R. Karl and S. Otto, Process for the Manufacture of 2-Chloroethane-Phosphonic acid: GB patent, 1373513 (1974).
D.I. Randall and C. Vogel, Preparation of 2-Haloethylphosphonic Acid: US Patent, 3808265 (1974).
D.I. Randall and R.W. Wynn, Mono-2-haloethyl Esters of 2-Haloethanephosphonic Acid: US Patent, 3626037 (1971).
J.E. Drach and B.J. Pendell, Process for the Manufacture of Aliphatic Phosphonic Acids: US Patent, 4064163 (1977).
K.W. Young and J.J. Zullo, Process for the Production of Aliphatic Phosphonic Acid: US Patent, 4728466 (1988).
L. Cauret, J.C. Brosse, D. Derouet and H. De Livonnière, Synth. Commun., 27, 647 (1997).
L.R. An, C.H. Wang and M.Q. Li, Jiangsu Agrochemicals, 4, 21 (1998).
GC internal standard method to measure content of ethephon: The ethephon was firstly converted completely into methyl ester by diazonium methane to give dimethyl 2-chloroethyl phosphonate (5), which content can be determined by GC through 10%SE-30 / Gas Chrom Q chromatography using p-nitrochlorobenzene as internal standard solution Through this way, the content of ethephon could be measured.