5-chloro-6-iodo-2,3-dihydro-1H-1,3-benzodiazole-2-thione synthesis
- Product Name:5-chloro-6-iodo-2,3-dihydro-1H-1,3-benzodiazole-2-thione
- CAS Number:1219741-21-5
- Molecular formula:C7H4ClIN2S
- Molecular Weight:310.54
75-15-0
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Yield:1219741-21-5 80%
Reaction Conditions:
with potassium hydroxide in ethanol;water; for 3 h;Inert atmosphere;Reflux;
Steps:
From this, a 100-mL round-bottom flask purged and maintained with an inert atmosphere of nitrogen. A solution of 4-chloro-5-iodobenzene-1,2-diamine (2.69 g, 10.02 mmol, 1.00 equiv) in ethanol (50 mL), CS2 (6 g, 78.95 mmol, 8.00 equiv) and potassium hydroxide (1.68 g, 30.00 mmol, 3.00 equiv) was placed into the flask. The resulting solution was heated to reflux for 3 h. The resulting mixture was concentrated under vacuum. The resulting solution was diluted with 100 mL of H2O. The resulting solution was extracted with 3×100 mL of ethyl acetate and the organic layers combined. The resulting mixture was washed with 100 mL of brine. The mixture was dried over anhydrous sodium sulfate and concentrated under vacuum. This resulted in 2.5 g (80%) of 5-chloro-6-iodo-2,3-dihydro-1H-1,3-benzodiazole-2-thione as a brown solid.
References:
US2013/281392,2013,A1 Location in patent:Paragraph 0148
1219741-20-4
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1219741-21-5
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1635-61-6
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1219741-21-5
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335349-57-0
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1219741-21-5
41 suppliers
$30.00/100mg