3,3-Dimethyl-1-(trifluoromethylthio)-1,2-benziodoxole, 95% synthesis
- Product Name:3,3-Dimethyl-1-(trifluoromethylthio)-1,2-benziodoxole, 95%
- CAS Number:1584705-82-7
- Molecular formula:C10H10F3IOS
- Molecular Weight:362.15
69352-04-1
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Yield:1584705-82-7 43%
Reaction Conditions:
at 50; for 1 h;Schlenk technique;Inert atmosphere;Sealed tube;
Steps:
5.2. General procedure for the preparation of reagent 3
AgSCF3 (3.5 g, 16.8 mmol), 1 chloro-1,3-dihydro-3,3-dimethyl-1,2-benziodoxole (5.0 g, 16.8 mmol) were placed into an oven-dried 100 mL Schlenk tube that is equipped with a stirring barunder Ar. The tube was quickly sealed with a rubber stopper andthe reaction was stirred at 50 8C for 1.0 h. Then 100 mL ofpetroleum ether was added, Filtration of the precipitated AgCl,followed by removal of the solvent gave a pale yellow oil. Theresidue was puried by ash chromatography on silica gel(Rf = 0.95, petroleum ether) to give reagent 3 (2.6 g, 43% yield)as a colorless oil.
References:
Ma, Bingqing;Shao, Xinxin;Shen, Qilong [Journal of Fluorine Chemistry,2015,vol. 171,p. 73 - 77]
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