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Triphosgene synthesis
- Product Name:Triphosgene
- CAS Number:32315-10-9
- Molecular formula:C3Cl6O3
- Molecular Weight:296.73
CH3OCO2CH3 + 6 Cl2 → CCl3OCO2CCl3 + 6 HCl
Triphosgene can be easily recrystallized from hot hexanes.
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594-42-3
2 suppliers
$74.00/25g
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32315-10-9
419 suppliers
$10.00/1g
Yield:-
Reaction Conditions:
with sulfur dioxide in dichloromethane;water at 10; for 4 h;
Steps:
12
Example 12To a glass reactor having a central vertical stirrer, a vertical condenser & a dip tube for passing chlorine gas, was charged 730 ml of 3N HC1 in 83.4gm of carbon disulfide, 388gm chlorine gas bubbled over 10 hrs at 24- 25°C. Reaction was terminated when carbon disulfide was < 1%. Trichloromethylsulfenyl chloride, 193 gm was obtained after work up & fractionation.Trichloromethylsulfenyl chloride (193 gm) was added in to a mixture of 500 gm water & 100 ml methylene dichloride, along with 83gm Sulfur dioxide gas at 10°C, over a period of 4 hrs. Reaction was terminated, when trichloromethyl sulfenyl chloride was <1%. Layer separation gave 228 g of thiophosgene which was added to a stirred mixture of 175 gm activated KF, 1 10 gm ortho-chlorobenzyl chloride and 340 gm spherogel (with 2mm diameter), at 60°C, over a period of 3hrs & further maintained at 60°C for 2 hrs gave 98% conversion. ortho-Chlorobenzyl trifluoromethylsulfide (138 gms) was isolated by filtration, followed by distillation, which was added to 500 ml methylene chloride, cooled to 0 to 10°C & 41 gm chlorine gas was bubbled into it, the reaction was maintained for 2 hrs & then heated slowly to 40-45°C. Generated trifluoromethylsulfenyl chloride was passed in to a solution of 5-amino-3-cyano-l-(2,6-dichloro-4- trifluoromethyl phenyl)-pyrazole in methylene dichloride to get 225 g of 5- amino-l-(2,6-dichloro-4-trifluoromethylphenyl)-3-cyano-4-trifluoromethyl thiopyrazole.
References:
WO2011/107998,2011,A1 Location in patent:Page/Page column 22-23
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616-38-6
688 suppliers
$5.00/5G
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32315-10-9
419 suppliers
$10.00/1g
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101970-86-9
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32315-10-9
419 suppliers
$10.00/1g
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207804-71-5
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32315-10-9
419 suppliers
$10.00/1g