Method for purifying high-purity phenyl ethyl malonate

A technology of diethyl phenylmalonate and ethyl acetate, which is applied in the field of purification of high-purity diethyl phenylmalonate, which can solve problems such as difficult to remove, affect the quality of downstream drug production, and difficult to separate
CN101633619BActive Publication Date: 2012-06-20南通森萱药业有限公司
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
南通森萱药业有限公司
Publication Date
2012-06-20

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Abstract

The invention relates to a method for purifying phenyl ethyl malonate, comprising the following steps: dissolving coarse phenyl ethyl malonate into a nonpolar solvent; decoloring by active carbon; filtering; mixing and crystallizing at the temperature of -10 DEG C to -5 DEG C; filtering to obtain a first filter cake; decompressing and recovering the solvent by the first filter cake to obtain colorless oil liquid as a fine product; dissolving the fine product into the nonpolar solvent; stirring and crystallizing at the temperature of -10 DEG C to -5 DEG C; filtering to obtain a second filter cake; decompressing the second cake to recover the solvent; and obtaining colorless transparent liquid as a phenyl ethyl malonate pure product. The purity of the phenyl ethyl malonate is greater than or equal to 99.5 percent, 2-phenyl-2-ethyl malonate impurities are less than 0.1 percent, and the total yield is greater than 90.0 percent.
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Description

technical field

[0001] The invention relates to a method for purifying high-purity diethyl phenylmalonate Background technique

[0002] Diethyl phenylmalonate is an important pharmaceutical intermediate, its structural formula is as follows:

[0003]

[0004] Its properties are colorless transparent liquid at normal temperature, b.p.160℃ / 5mmHg, F.P.15℃.

[0005] It is mainly used in

[0006] (1) the application of cephalosporin drug, its reaction formula is as follows:

[0007]

[0008] (2) Application in other medicines.

[0009]

[0010] The main impurity of diethyl phenylmalonate in the synthesis process is ethyl 2-phenylbutyrate (I), ethyl phenylacetate (II), diethyl 2-phenyl-2-ethylmalonate Ester (III), its structural formula is as follows:

[0011]

[0012] Among them, impurity (III) introduces "ethyl" at the α-position of diethyl phenylmalonate, which has a greater impact on the application of diethyl phenylmalonate in drug synthesis, and will import ...

Claims

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