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Process for preparing 1-naphtylacetonitrile via potassium cyanide and 1-chloromethyl naphthalene

A technology of chloromethylnaphthalene and potassium cyanide, which is applied in the field of preparing 1-naphthaleneacetonitrile, can solve the problems of waste of resources, unsatisfactory homogeneity of 1-naphthaleneacetonitrile, and low success rate, so as to reduce adverse effects and improve preparation success rate, improve the effect of stability

Inactive Publication Date: 2017-08-11
枣阳市残联福利生物化工厂
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] 1-naphthaleneacetonitrile is an important intermediate for the synthesis of agomelatine. For this reason, the preparation of 1-naphthaleneacetonitrile has also attracted much attention. The existing preparation processes are directly synthesized, and the prepared 1-naphthalene Acetonitrile is not ideal in homogeneity, and the success rate of synthesis is not high, often causing unnecessary waste of resources

Method used

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Effect test

Embodiment 1

[0021] The present invention proposes a kind of technique that prepares 1-naphthalene acetonitrile by potassium cyanide and 1-chloromethyl naphthalene, comprises the steps:

[0022] S1. Potassium cyanide, 1-chloromethylnaphthalene and protective agent are selected as the main raw materials, and the weight ratio of potassium cyanide and 1-chloromethylnaphthalene is 1:1.5, and the main raw materials are sealed and preserved;

[0023] S2. Potassium cyanide is placed in a heating container, and after the temperature of potassium cyanide is maintained at 40 degrees Celsius, it is moved to a constant temperature container;

[0024] S3, 1-chloromethylnaphthalene is placed in the heating container, and after the temperature of 1-chloromethylnaphthalene is maintained at 30 degrees Celsius, it is moved to a constant temperature container;

[0025] S4, the potassium cyanide treated in S2 is placed in the reactor, and the 1-chloromethylnaphthalene treated in S3 is slowly added dropwise to...

Embodiment 2

[0036] The present invention proposes a kind of technique that prepares 1-naphthalene acetonitrile by potassium cyanide and 1-chloromethyl naphthalene, comprises the steps:

[0037] S1. Potassium cyanide, 1-chloromethylnaphthalene and protective agent are selected as the main raw materials, and the weight ratio of potassium cyanide and 1-chloromethylnaphthalene is 1:1.5, and the main raw materials are sealed and preserved;

[0038] S2. Potassium cyanide is placed in a heating container, and after the temperature of potassium cyanide is maintained at 43 degrees Celsius, it is moved to a constant temperature container;

[0039] S3, 1-chloromethylnaphthalene is placed in the heating container, and after the temperature of 1-chloromethylnaphthalene is maintained at 32 degrees Celsius, it is moved to a constant temperature container;

[0040] S4, the potassium cyanide treated in S2 is placed in the reactor, and the 1-chloromethylnaphthalene treated in S3 is slowly added dropwise to...

Embodiment 3

[0051] The present invention proposes a kind of technique that prepares 1-naphthalene acetonitrile by potassium cyanide and 1-chloromethyl naphthalene, comprises the steps:

[0052] S1. Potassium cyanide, 1-chloromethylnaphthalene and protective agent are selected as the main raw materials, and the weight ratio of potassium cyanide and 1-chloromethylnaphthalene is 1:1.5, and the main raw materials are sealed and preserved;

[0053] S2. Potassium cyanide is placed in a heating container, and after the temperature of potassium cyanide is maintained at 47 degrees Celsius, it is moved to a constant temperature container;

[0054] S3, 1-chloromethylnaphthalene is placed in the heating container, and after the temperature of 1-chloromethylnaphthalene is maintained at 34 degrees Celsius, it is moved to a constant temperature container;

[0055] S4, the potassium cyanide treated in S2 is placed in the reactor, and the 1-chloromethylnaphthalene treated in S3 is slowly added dropwise to...

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Abstract

The invention discloses a process for preparing 1-naphtylacetonitrile via potassium cyanide and 1-chloromethyl naphthalene; the process comprises the steps of selecting potassium cyanide, 1-chloromethyl naphthalene, and a protectant as main materials, adding the treated potassium cyanide into a reactor, dropwise adding the treated 1-chloromethyl naphthalene slowly into the reactor holding the potassium cyanide, with the temperature of the reactor kept at 55-70 DEG C, mixing and stirring after dropwise adding, heating to 90-120 DEG C, adding a catalyst into the mixed solution, allowing reacting at 75-80 DEG C for 30-45 s, transferring into a drying device, drying at 200-240 DEG C, adding the protectant into the reacted liquid, concentrating the reacted liquid, crystallizing to obtain white powder, extracting the white powder, and recrystallizing to obtain 1-naphtylacetonitrile. The process has the advantages that preparation stability is effectively improved, the preparation method is reliable and the process is suitable for late large-batch production.

Description

technical field [0001] The invention relates to the technical field of chemical substance synthesis, in particular to a process for preparing 1-naphthaleneacetonitrile from potassium cyanide and 1-chloromethylnaphthalene. Background technique [0002] 1-naphthaleneacetonitrile is an important intermediate for the synthesis of agomelatine. For this reason, the preparation of 1-naphthaleneacetonitrile has also attracted much attention. The existing preparation processes are directly synthesized, and the prepared 1-naphthalene The homogeneity of acetonitrile is not ideal, and the success rate of synthesis is not high, often causing unnecessary waste of resources. Therefore, a process for preparing 1-naphthaleneacetonitrile from potassium cyanide and 1-chloromethylnaphthalene was proposed, and the existing preparation process was optimized. Contents of the invention [0003] The present invention proposes a process for preparing 1-naphthaleneacetonitrile by potassium cyanide ...

Claims

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Application Information

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IPC IPC(8): C07C253/14C07C255/33C07C17/263C07C22/04
CPCC07C253/14C07C17/263C07C255/33C07C22/04
Inventor 曹亮
Owner 枣阳市残联福利生物化工厂
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