阅读说明：本技术 一种1,3-二氨基硫脲的合成方法 (Synthetic method of 1, 3-diaminothiourea ) 是由 陈健龙 金璐仪 于 2021-09-30 设计创作，主要内容包括：本发明属于医药中间体技术领域,具体涉及一种1,3-二氨基硫脲的合成方法。本发明采用水合肼、二硫化碳作为原料,通过使用巯基乙醇作为催化剂,通过加入麻黄碱作为催化剂用助剂,提高催化效能,加快反应速度,缩短了反应时效,提高了反应效率。(The invention belongs to the technical field of medical intermediates, and particularly relates to a synthetic method of 1, 3-diaminothiourea. The invention adopts hydrazine hydrate and carbon disulfide as raw materials, adopts mercaptoethanol as a catalyst, and adds ephedrine as an auxiliary agent for the catalyst, thereby improving the catalytic efficiency, accelerating the reaction speed, shortening the reaction time and improving the reaction efficiency.)

1. A synthesis method of 1, 3-diaminothiourea is characterized in that hydrazine hydrate and sulfur dioxide react at 63-66 ℃ under the action of a catalyst and an auxiliary agent to obtain a product 1, 3-diaminothiourea;

the catalyst is mercaptoethanol, and the auxiliary agent is ephedrine.

2. The method for synthesizing 1, 3-diaminothiourea according to claim 1, characterized in that the method for synthesizing is specifically:

(1) putting hydrazine hydrate, mercaptoethanol and water into a reactor, setting the temperature to be 8-10 ℃, adding carbon disulfide and ephedrine, and carrying out heat preservation reaction;

(2) and after the reaction is finished, heating to 65-68 ℃, and reacting to obtain the 1, 3-diaminothiourea.

3. The method for synthesizing 1, 3-diaminothiourea according to claim 2, characterized in that the molar ratio of hydrazine hydrate, mercaptoethanol, carbon disulfide and ephedrine is 4-6: 0.3:2: 0.1.

Technical Field

The invention belongs to the technical field of medical intermediates, and particularly relates to a synthetic method of 1, 3-diaminothiourea.

Background

1, 3-diaminothiourea (TCH for short) is an important organic synthesis intermediate, has wide application in the synthesis of some heterocyclic medicines and pesticides, and some metal derivatives thereof also have great application value. Then, in the prior art, the reaction time is long and the yield is low.

Disclosure of Invention

The invention aims to solve the technical problem of providing a method for synthesizing 1, 3-diaminothiourea.

In order to solve the technical problems, the invention adopts the following technical scheme:

a synthetic method of 1, 3-diaminothiourea comprises the steps of reacting hydrazine hydrate and sulfur dioxide at 63-66 ℃ under the action of a catalyst and an auxiliary agent to obtain a product 1, 3-diaminothiourea;

the catalyst is mercaptoethanol, and the auxiliary agent is ephedrine.

Preferably, the method for synthesizing comprises the following specific steps:

(1) putting hydrazine hydrate, mercaptoethanol and water into a reactor, setting the temperature to be 8-10 ℃, adding carbon disulfide and ephedrine, and carrying out heat preservation reaction;

(2) and after the reaction is finished, heating to 65-68 ℃, and reacting to obtain the 1, 3-diaminothiourea.

Preferably, the molar ratio of hydrazine hydrate to mercaptoethanol to carbon disulfide to ephedrine is 4-6: 0.3:2: 0.1.

Compared with other methods, the method has the beneficial technical effects that:

the invention adopts hydrazine hydrate and carbon disulfide as raw materials, adopts mercaptoethanol as a catalyst, and adds ephedrine as an auxiliary agent for the catalyst, thereby improving the catalytic efficiency, accelerating the reaction speed, shortening the reaction time and improving the reaction efficiency.

Detailed Description

The technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

A method for synthesizing 1, 3-diaminothiourea comprises the following steps:

(1) taking materials according to the molar ratio of hydrazine hydrate to mercaptoethanol to carbon disulfide to ephedrine of 4-6: 0.3:2:0.1, putting hydrazine hydrate into a reactor, adding mercaptoethanol, setting the temperature to be 8-10 ℃, adding carbon disulfide and ephedrine, and carrying out heat preservation reaction for 2 hours;

(2) heating the temperature of the reaction kettle to 65-68 ℃, preserving the temperature for 6h, spraying alkaline water on tail gas hydrogen sulfide for reaction to generate sodium sulfide, spraying water, absorbing and discharging active carbon, then cooling to about 20-25 ℃, starting discharging and suction filtering, washing with water, then suction filtering, drying through drying equipment after suction filtering, and packaging to obtain the 1, 3-diaminothiourea.

Example 1

A method for synthesizing 1, 3-diaminothiourea comprises the following steps:

(1) taking the hydrazine hydrate, mercaptoethanol, carbon disulfide and ephedrine according to the molar ratio of 4:0.3:2:0.1, putting the hydrazine hydrate into a reactor, adding mercaptoethanol, setting the temperature to be 8-10 ℃, adding the carbon disulfide and the ephedrine, and carrying out heat preservation reaction for 2 hours;

(2) heating the temperature of the reaction kettle to 65-68 ℃, keeping the temperature for 6h, spraying alkaline water on tail gas hydrogen sulfide for reaction to generate sodium sulfide, spraying water, absorbing and discharging active carbon, then cooling to about 20-25 ℃, starting discharging and suction filtering, washing with water, then suction filtering, drying by drying equipment after suction filtering, and packaging to obtain the 1, 3-diaminothiourea, wherein the calculated yield is 98.6%, and the purity is 98.8%.

Example 2

A method for synthesizing 1, 3-diaminothiourea comprises the following steps:

(1) taking the hydrazine hydrate, mercaptoethanol, carbon disulfide and ephedrine according to the molar ratio of 6:0.3:2:0.1, putting the hydrazine hydrate into a reactor, adding mercaptoethanol, setting the temperature to be 8-10 ℃, adding the carbon disulfide and the ephedrine, and carrying out heat preservation reaction for 2 hours;

(2) heating the temperature of the reaction kettle to 65-68 ℃, preserving the temperature for 6h, spraying alkaline water on tail gas hydrogen sulfide for reaction to generate sodium sulfide, spraying water, absorbing and discharging active carbon, then cooling to about 20-25 ℃, starting discharging and suction filtering, washing with water, then suction filtering, drying by drying equipment after suction filtering, and packaging to obtain the 1, 3-diaminothiourea, wherein the calculated yield is 98.9%, and the purity is 99.1%.

Example 3

A method for synthesizing 1, 3-diaminothiourea comprises the following steps:

(1) taking the hydrazine hydrate, mercaptoethanol, carbon disulfide and ephedrine according to the molar ratio of 5:0.3:2:0.1, putting the hydrazine hydrate into a reactor, adding mercaptoethanol, setting the temperature to be 8-10 ℃, adding the carbon disulfide and the ephedrine, and carrying out heat preservation reaction for 2 hours;

(2) heating the temperature of the reaction kettle to 65-68 ℃, preserving the temperature for 6h, spraying alkaline water on tail gas hydrogen sulfide for reaction to generate sodium sulfide, spraying water, absorbing and discharging active carbon, then cooling to about 20-25 ℃, starting discharging and suction filtering, washing with water, then suction filtering, drying by drying equipment after suction filtering, and packaging to obtain the 1, 3-diaminothiourea, wherein the calculated yield is 98.2%, and the purity is 98.1%. .

Example 4

A method for synthesizing 1, 3-diaminothiourea comprises the following steps:

(1) taking materials according to the molar ratio of hydrazine hydrate to mercaptoethanol to carbon disulfide of 6:0.3:2, putting hydrazine hydrate into a reactor, adding mercaptoethanol, setting the temperature to be 8-10 ℃, adding carbon disulfide, and reacting for 3 hours in a heat preservation manner;

(2) heating the temperature of the reaction kettle to 65-68 ℃, keeping the temperature for 16h, spraying alkaline water on tail gas hydrogen sulfide for reaction to generate sodium sulfide, spraying water, absorbing and discharging active carbon, then cooling to about 20-25 ℃, starting discharging and suction filtering, washing with water, then suction filtering, drying by drying equipment after suction filtering, and packaging to obtain the 1, 3-diaminothiourea, wherein the calculated yield is 98.9%, and the purity is 99.1%.

Example 5

A method for synthesizing 1, 3-diaminothiourea comprises the following steps:

(1) taking materials according to the molar ratio of hydrazine hydrate to carbon disulfide of 4-6: 2, putting hydrazine hydrate into a reactor, setting the temperature to be 8-10 ℃, adding carbon disulfide, and carrying out heat preservation reaction for 6 hours;

(2) heating the temperature of the reaction kettle to 65-68 ℃, preserving the temperature for 22 hours, spraying alkaline water on tail gas hydrogen sulfide for reaction to generate sodium sulfide, spraying water, absorbing and discharging active carbon, then cooling to about 20-25 ℃, starting discharging and suction filtering, washing with water, then suction filtering, drying by drying equipment after suction filtering, and packaging to obtain the 1, 3-diaminothiourea, wherein the calculated yield is 36.2%, and the purity is 73.6%.

The present invention has been further described with reference to specific embodiments, but it should be understood that the detailed description should not be construed as limiting the spirit and scope of the present invention, and various modifications made to the above-described embodiments by those of ordinary skill in the art after reading this specification are within the scope of the present invention.