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ChemicalBook CAS DataBase List Ethoxycarbonyl Isothiocyanate

Ethoxycarbonyl Isothiocyanate synthesis

6synthesis methods
-

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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