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CAS No. : | 611-19-8 | MDL No. : | MFCD00000893 |
Formula : | C7H6Cl2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | BASMANVIUSSIIM-UHFFFAOYSA-N |
M.W : | 161.03 | Pubchem ID : | 11906 |
Synonyms : |
|
Signal Word: | Danger | Class: | 6.1 |
Precautionary Statements: | P210-P264-P270-P271-P272-P280-P303+P361+P353-P304+P340-P305+P351+P338-P310-P330-P331-P370+P378-P362+P364-P403+P233-P501 | UN#: | 2235 |
Hazard Statements: | H227-H314-H317-H335-H410-H302+H312+H332 | Packing Group: | Ⅲ |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
815 kg | Stage #1: With sodium carbonate In water at 85℃; for 2 h; Large scale Stage #2: at 85℃; Large scale |
1000 kg of water was charged to a 4000 L reactor, then 460 kg of 4, 4-dimethyl-3-isoxazolidinone was added. The resulting solution was stirred at room temperature for 1 h. Thereafter, 383 kg of Na2C03 was added in small portions. The temperature of the resulting mixture was raised to 85°C and the mixture stirred at this temperature for 2 h. Thereafter, 672 kg of 2-chlorobenzyl chloride was added dropwise over a period of 5 h at 85°C. After the addition was completed, the resulting solution was stirred at the same temperature until the reaction had completed. The resulting mixture was cooled to room tempertaure and 800 kg of dichloromethane was added to the reactor. The resulting mixture was stirred at room temperature for 15 h. Thereafter, the aqueous phase was separated, extracted with dichloromethane (3 times). Dichloromethane was recovered by distillation and then 2000 kg of hexane was added into the reactor. The resulting mixture was refluxed for 1 h, then cooled to 10 to 15°C and stirred for another 1 h. The solid material was isolated by filtration. The solid was washed with hexanes several times and dried under high vacuum to give pure clomazone Technical (815 kg, Purity: 96percent). Similar results are obtained using sodium hydroxide as the base, in place of sodium carbonate. |
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