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Prepn of N-methyl-2-naphthyl carbamate

A technology of naphthyl carbamate and methyl group is applied in the field of preparation of chemical substance N-methyl-2-naphthyl carbamate, which can solve the problem of high production cost, reduce material cost and highlight substantial Features, Significantly Improved Effects

Inactive Publication Date: 2004-12-01
INST OF ZOOLOGY CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its disadvantage is the use of solvent medium, high production cost

Method used

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  • Prepn of N-methyl-2-naphthyl carbamate
  • Prepn of N-methyl-2-naphthyl carbamate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Under the stirring condition of 8-10 circles per minute, add 9.2g (0.23M) sodium hydroxide, 125g water, 29g (0.2M) 2-naphthol into a 1000ml three-necked flask to make an aqueous solution of phenolic sodium salt;

[0017] At 0-10°C, add 23g (0.25M) carbamoyl chloride, and at the same time, add 125ml of an aqueous solution containing 2g (0.05M) sodium hydroxide dropwise into the three-necked flask, and finish adding dropwise in 30 minutes. Continue the reaction at the above temperature 1 hour;

[0018] After the reaction is completed, filter with suction, wash with water and air-dry to obtain N-methyl-2-naphthyl carbamate crystals;

[0019] The yield of N-methyl-2-naphthyl carbamate in this example is 95%, and the yield can reach more than 90% in industrial practice.

Embodiment 2

[0021] Under the stirring condition of 8-10 circles per minute, add 10g (0.25M) sodium hydroxide, 130g water, 29g (0.2M) 2-naphthol into a 1000ml three-necked flask to make an aqueous solution of phenolic sodium salt;

[0022] At -5-0°C, add 25.1g (0.27M) carbamoyl chloride, and at the same time add 125ml of an aqueous solution containing 4g (0.1M) sodium hydroxide dropwise to the three-necked flask, and drop it in 30 minutes. At the above temperature Continue to react for 1 hour;

[0023] After completion of the reaction, suction filtration, washing with water and air-drying gave N-methyl-2-naphthyl carbamate crystals; the yield of N-methyl-2-naphthyl carbamate in this example was 95%. , and the yield can reach more than 90% in industrialized implementation.

Embodiment 3

[0025] Under the stirring condition of 8-10 circles per minute, add 12g (0.3M) sodium hydroxide, 150g water, 29g (0.2M) 2-naphthol into a 1000ml three-necked flask to make an aqueous solution of phenolic sodium salt;

[0026] At 5-10°C, add 28.0g (0.3M) carbamoyl chloride, and at the same time, add 125ml of an aqueous solution containing 5g (0.125M) sodium hydroxide dropwise into the three-necked flask, and finish adding dropwise in 30 minutes. Continue at the above temperature React for 1 hour;

[0027] After the reaction is completed, filter with suction, wash with water and air-dry to obtain N-methyl-2-naphthyl carbamate crystals;

[0028] The yield of N-methyl-2-naphthyl carbamate in this example is 95%, and the yield can reach more than 95% in industrial practice.

[0029] raw material

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Abstract

The preparation process of N-methyl-2-naphthyl carbamate incldues dissolving 2-naphthol in water solution of sodium hydroxide; adding solid methyamino formyl chloride at room temperature while stirring to produce solid N-methyl-2-naphthyl carbamate dispersed in the liquid medium; sucking filtering, water washing and air drying to obtain crystal N-methyl-2-naphthyl carbamate. The reactant ratio among 2-naphthol, sodium hydroxide and methyamino formyl chloride is 1 to 1.3 to 1.3. The present invention has low cost in material and low reaction temperature.

Description

technical field [0001] The invention belongs to the preparation method of chemical substance N-methyl-2-naphthyl carbamate. Background technique [0002] The preparation method of N-methyl-2-naphthyl carbamate in the prior art is prepared by reacting 2-naphthol and carbamoyl chloride in a cumene (cumene) solution at 80°C. Its disadvantage is the use of solvent medium and high production cost. Contents of the invention [0003] The purpose of this invention is to propose a new method for preparing N-methyl-2-naphthyl carbamate, which can reduce costs and overcome the shortcomings of the prior art. [0004] Technical scheme of the present invention is as follows: [0005] The preparation method of N-methyl-2-naphthyl carbamate provided by the invention is characterized in that the steps are as follows: [0006] 1) 2-naphthol is dissolved in aqueous sodium hydroxide solution to make sodium phenate solution; [0007] 2) U...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C269/00C07C271/04
Inventor 曾益良任连奎秦小薇
Owner INST OF ZOOLOGY CHINESE ACAD OF SCI