Ethoxycarbonyl Isothiocyanate synthesis
- Product Name:Ethoxycarbonyl Isothiocyanate
- CAS Number:16182-04-0
- Molecular formula:C4H5NO2S
- Molecular Weight:131.15
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16182-04-0
Example 1: Preparation of ethoxycarbonyl isothiocyanate To a 1 liter jacketed reactor was added sodium thiocyanate (39.1 g, 0.48 mol) and 310 g of toluene. After heating the mixture to 30°C, pyridine (0.4 g, 0.005 mol) and water (0.9 g, 0.05 mol) were added sequentially. Subsequently, ethyl chloroformate (52.9 g, 0.49 mol) was added slowly and dropwise to the reaction system over 40 minutes. The reaction solution was maintained under stirring for 3 hours, during which time the progress of the reaction was monitored by gas chromatography (GC) to confirm that the ethyl chloroformate was almost completely consumed. Upon completion of the reaction, the reaction solution was filtered and analyzed by gas chromatography combined with quantitative internal standard method and the yield of ethoxycarbonyl isothiocyanate was measured to be 99%.
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Yield:16182-04-0 99%
Reaction Conditions:
with pyridine in water;toluene
Steps:
1 Preparation of ethoxycarbonyl isothiocyanate
Example 1
Preparation of ethoxycarbonyl isothiocyanate
A 1-liter (L) jacketed reactor was charged with sodium thiocyanate (39.1 grams (g), 0.48 moles (mol)) and 310 g of toluene.
The solution was heated to 30° C. and treated with pyridine (0.4 g, 0.005 mol) and water (0.9 g, 0.05 mol).
Then ethyl chloroformate (52.9 g, 0.49 mol) was added drop-wise to the solution over 40 minutes (min).
The solution was left to stir for 3 hours (h), at which time nearly all the ethyl chloroformate had been consumed as determined by gas chromatography (GC).
The solution was then filtered and analyzed by GC affording the final product in 99% yield as determined using a quantitative internal standard method.
References:
Dow AgroSciences LLC;Fisk, Jason S.;Bland, Douglas C.;Frycek, George J. US2014/100381, 2014, A1 Location in patent:Page/Page column
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463 suppliers
$13.50/100G
541-41-3
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$19.39/5g
16182-04-0
230 suppliers
$10.00/1g
541-41-3
0 suppliers
$19.39/5g
16182-04-0
230 suppliers
$10.00/1g
