A kind of synthetic method of imidate derivative
A technology of imidate and synthesis method, which is applied in the direction of organic chemistry, can solve the problems of harsh reaction conditions and single type of imidate, and achieve the effect of easy purification, rich structure and mild reaction conditions
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Embodiment 1
[0025]
[0026] A kind of synthetic method of imidate derivative, its concrete steps are as follows:
[0027] (1) Taking phenoxynitrile and ethyl acetoacetate as raw materials, ether as a solvent, according to the ratio of phenoxynitrile mmol: ethyl acetoacetate mmol: ethyl ether milliliter ratio of 1.2: 1: 2, in the reactor Phenoxynitrile (129.8 μL, 1.2 mmol), ethyl acetoacetate (127.6 μL, 1.0 mmol) and diethyl ether (2.0 mL) were added successively. After the addition was complete, the reaction was continued to stir at room temperature for 40 hours.
[0028] (2) After step (1) is completed, the reaction solution of the imidate derivative prepared in step (1) is concentrated by rotary evaporation, and the concentrated solution is collected; the concentrated solution is purified by silica gel column chromatography, washed with The liquid was removed for elution, and the effluent from the silica gel column chromatography was concentrated by rotary evaporation and sucked to d...
Embodiment 2
[0031]
[0032] A kind of synthetic method of imidate derivative, its concrete steps are with embodiment 1, wherein:
[0033] In step (1), p-ethylphenoxynitrile and ethyl acetoacetate are used as raw materials, and ether is used as a solvent, and the ratio of p-ethylphenoxynitrile mmol: ethyl acetoacetate mmol: ether ml is 1.2:1 : 2 ratio, p-ethylphenoxynitrile (88.2mg, 0.6mmol), ethyl acetoacetate (64μL, 0.5mmol) and diethyl ether (1.0mL) were added successively in the reactor, and the addition was completed, and the stirring was continued at room temperature React for 44 hours.
[0034] In step (2), the eluent was a mixture of ethyl acetate:petroleum ether with a volume ratio of 1:(2-20), and imidate 3b was obtained as a white solid (57.6 mg, yield 42%).
Embodiment 3
[0036]
[0037] A kind of synthetic method of imidate derivative, its concrete steps are with embodiment 1, wherein:
[0038] In step (1), p-methoxyphenoxynitrile and ethyl acetoacetate are used as raw materials, and ether is used as a solvent, and the ratio of p-methoxyphenoxynitrile mmol: ethyl acetoacetate mmol: ether milliliter is 1.2 : The ratio of 1:2, add p-methoxyphenoxynitrile (178.8mg, 1.2mmol), ethyl acetoacetate (127.6μL, 1.0mmol) and diethyl ether (2.0mL) successively in the reactor, after addition is completed, in The stirring reaction was continued at room temperature for 45 hours.
[0039] In step (2), the eluent is a mixture of ethyl acetate:petroleum ether with a volume ratio of 1:(2-20), and imidate 3c (210.6mg, yield 76%) is obtained as a colorless viscous liquid .
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