Purification method of NN dimethyl acetamide

The technology of a dimethylacetamide and a purification method is applied in the field of purification of NN dimethylacetamide, can solve the problem that NN-dimethylacetamide cannot be used for the detection of residual solvent of nadolamine, and achieves high purity, The effect of increasing the number of plates and improving the effect

Pending Publication Date: 2019-11-22
新乡双鹭药业有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In view of this, the application provides a purification method of NN-dimethylacetamide, which solves the problem that the existing NN-dimethylacetamide cannot be used for the detection of residual solvents of lenatoamine. The high-purity NN-dimethylacetamide prepared by the present invention NN-Dimethylacetamide can not only be used for the detection of residual solvents of lenadolamine, but also meet the detection requirements of all gas phases

Method used

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  • Purification method of NN dimethyl acetamide
  • Purification method of NN dimethyl acetamide
  • Purification method of NN dimethyl acetamide

Examples

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Embodiment 1

[0032] A purification method of NN-dimethylacetamide, comprising the following steps:

[0033] (1) The round-bottomed flask equipped with 2L industrial grade NN-dimethylacetamide is connected to a condenser connected to a water circulation vacuum pump, placed in an electric heating mantle, and the other end of the condenser is connected to the collection device through a packed column;

[0034] (2) Set the ultra-high temperature of the electric heating jacket to 200°C;

[0035] (3) Turn on the power supply of the water circulation vacuum pump, control the vacuum degree to be -0.080, and keep the boiling temperature of NN-dimethylacetamide in the container at 115°C;

[0036] (4) When there is liquid dripping in the condenser, perform total reflux for 30 minutes, turn on the power supply of the collection device after the total reflux, and the purified NN-dimethylacetamide can be collected;

[0037] (5) The collection of NN-dimethylacetamide in step (4) is carried out in four s...

Embodiment 2

[0044] A purification method of NN-dimethylacetamide, comprising the following steps:

[0045] (1) The round-bottomed flask equipped with 2L industrial grade NN-dimethylacetamide is connected to a condenser connected to a water circulation vacuum pump, placed in an electric heating mantle, and the other end of the condenser is connected to the collection device through a packed column;

[0046] (2) Set the ultra-high temperature of the electric heating jacket to 200°C;

[0047] (3) Turn on the power supply of the water circulation vacuum pump, control the vacuum degree to be -0.080, and keep the boiling temperature of NN-dimethylacetamide in the container at 120°C;

[0048] (4) When there is liquid dripping in the condenser, perform total reflux for 30 minutes, turn on the power supply of the collection device after the total reflux, and the purified NN-dimethylacetamide can be collected;

[0049] (5) The collection of NN-dimethylacetamide in step (4) is carried out in four s...

Embodiment 3

[0056] A purification method of NN-dimethylacetamide, comprising the following steps:

[0057] (1) The round-bottomed flask equipped with 2L industrial grade NN-dimethylacetamide is connected to a condenser connected to a water circulation vacuum pump, placed in an electric heating mantle, and the other end of the condenser is connected to the collection device through a packed column;

[0058] (2) Set the ultra-high temperature of the electric heating jacket to 200°C;

[0059] (3) Turn on the power supply of the water circulation vacuum pump, control the vacuum degree to be -0.080, and keep the boiling temperature of NN-dimethylacetamide in the container at 125°C;

[0060] (4) When there is liquid dripping in the condenser, perform total reflux for 30 minutes, turn on the power supply of the collection device after the total reflux, and the purified NN-dimethylacetamide can be collected;

[0061] (5) The collection of NN-dimethylacetamide in step (4) is carried out in four s...

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Abstract

The invention discloses a purification method of NN-dimethylacetamide, which is characterized by comprising the following steps of (1) connecting a container filled with the industrial-grade NN-dimethylacetamide with a condenser connected with a water circulating vacuum pump, placing the container in a heating device, and connecting the other end of the condenser with a collection device through apacked column; (2) setting the ultrahigh temperature of the heating device to be 200 DEG C; (3) turning on the power supply of the water circulation vacuum pump, controlling the vacuum degree to be -0.080 to -0.090, and keeping the boiling temperature of the NN-dimethylacetamide in the container to be 115 to 125 DEG C; and (4) carrying out total reflux when liquid drips in the condenser, and turning on the power supply of the collection device after total reflux so as to collect the purified NN-dimethylacetamide, wherein the collection of the NN-dimethylacetamide in the step (4) is divided into four stages, the volume ratio of the reagents collected in sequence is 7: 16: 8: 9, and the reagent collected at the third stage is the high-purity NN-dimethylacetamide.

Description

technical field [0001] The invention relates to the technical field of reagent purification, in particular to a method for purifying NN dimethylacetamide. Background technique [0002] Requirements for NN-dimethylacetamide in the detection of residual solvents of lenadolin: the peak height at 12.17 is about 2PA; the peak height at 13.29 is about 3PA; the absorption peaks at 12.17 and 13.29 are in the gas chromatogram of NN-dimethylacetamide The two main impurity peaks, and close to NN-dimethylacetyl, are not easy to separate by ordinary distillation. [0003] None of the existing GC-grade NN-dimethylacetamide, Merck GC-grade NN-dimethylacetamide, and industrial grade NN-dimethylacetamide can meet the requirements for the detection of lenadoamine residual solvents, such as figure 1 , figure 2 , image 3 shown. [0004] NN-Dimethylacetamide has strict requirements for NN-dimethylacetamide in the detection of residual solvents of lenalidomide. NN-Dimethylacetamide itself h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/24C07C233/05
CPCC07C231/24C07C233/05
Inventor 吕振培秦丽华任团军
Owner 新乡双鹭药业有限公司
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