5-Chloro-3-isopropyl-1,2,4-thiadiazole synthesis
- Product Name:5-Chloro-3-isopropyl-1,2,4-thiadiazole
- CAS Number:51302-12-6
- Molecular formula:C5H7ClN2S
- Molecular Weight:162.64
22007-68-7
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51302-12-6
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Yield:-
Reaction Conditions:
with sodium hydroxide in dichloromethane at 0 - 20; for 5.33333 h;
Steps:
8.A
To a mixture of 2-methyl propanimidamide hydrochloride (5.0 g, 40.8 mmol), trichloromethanesulfenyl chloride (7.14 g, 38.4 mmol) in methylene chloride (200 mL) at 0 °C was added dropwise an aqueous solution of sodium hydroxide (50%, 9.9 mL) over 20 minutes. The reaction mixture was stirred for 2 h at 0 °C and then was allowed to warm to room temperature, and stirred for an additional 3 h. Ice was added to the reaction mixture, the mixture was separated, and the aqueous layer was extracted with methylene chloride (3 x 25 mL). The combined organic extracts were dried over magnesium sulfate, filtered and concentrated under reduced pressure. The resulting residue was purified by medium pressure liquid chromatography (0 to 100% gradient of ethyl acetate in hexanes as eluant) to provide the title compound as a oil (3.8 g).
References:
WO2008/124092,2008,A2 Location in patent:Page/Page column 46
