Improved method for synthesizing amino formic acid ester compound
A technology of carbamate and oxime carbamate, which is applied in the field of preparing carbamate compounds, can solve undisclosed problems and achieve the effect of increasing the production rate
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Embodiment 1
[0031] This example illustrates the effectiveness of the catalyst of the present invention.
[0032] 1 g (4.9 mmol) of dibromoformaldoxime was charged in a 50 ml three-necked round-bottomed flask equipped with a stirring bar and a nitrogen atmosphere, and 10 g of dichloromethane containing 2% (by weight) of a suitable catalyst was added thereto. The mixture was stirred until the solids were all dissolved. Then 0.49 g (4.9 mmol) of n-butyl isocyanate was added to the flask. The reaction mixture was stirred at room temperature.
[0033] After 0.5 hours and 16 hours of reaction, a portion of the reaction mixture (50 mg) was taken out, and a portion of the mixture taken out was quenched with a 50 / 50 (v / v) hexane / ethyl acetate mixture, and then analyzed by GC to determine the formation of Percentage of N-n-butyldibromoformaldoxime carbamate and by-products. The identity of N-n-butyldibromoformaldoxime carbamate and by-products was determined by comparison with the compound's ana...
Embodiment 2
[0038] This example shows the range of catalysts used in the present invention.
[0039] Use the catalyst listed in Table 2 to repeat the process of Example 1 in indicated amounts. Sampling and analysis by the method of Example 1. The percent carbamate and by-products formed are reported in Table 2.
[0040] Table 2: Percent carbamate formation *NA=not analyzed
[0041] These data indicate that 0.5% by weight zinc acetylacetonate provides a purer carbamate in higher yield than other known catalysts.
Embodiment 3
[0043] This example illustrates some solvents suitable for use in the present invention.
[0044] Using the solvents listed in Table 3, the process of Example 1 was repeated with zinc acetylacetonate as the catalyst. After 0.5 hours and 16 hours of reaction, a reaction sample was taken out, and the sample was analyzed by GC for the amount of carbamate formed. The results are reported in Table 3.
[0045] Table 3: Percent carbamate formation *NA=not analyzed
[0046] These data indicate that some types of solvents are suitable for use in the process of the invention.
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