CN106588730B

CN106588730B - A kind of preparation method of Diallytrisin

Info

Publication number: CN106588730B
Application number: CN201611096479.9A
Authority: CN
Inventors: 杨亮; 杨位祥
Original assignee: Yoshida Spice Ltd By Share Ltd Shandong
Current assignee: Yoshida Spice Ltd By Share Ltd Shandong
Priority date: 2016-12-02
Filing date: 2016-12-02
Publication date: 2019-01-11
Anticipated expiration: 2036-12-02
Also published as: CN106588730A

Abstract

The invention discloses a kind of synthetic method is simple, raw material is easy to get, and reaction step is few, the preparation method of the high Diallytrisin of finished product content, comprising the following steps: 1) sodium hydrosulfide for taking 50 parts of NaHS that 0.6 mol is made with 100 parts of water is spare；2) 1000ml there-necked flask is taken, is added 280 parts of pure water, Bunte salt is made in 300 parts of the dodium thiosulfate of 1.2mol, 92 parts of the chloropropene of 1.2mol；3) 30 ~ 50 DEG C of temperature control stir lower a dropping step 1) prepared by 150 parts of sodium hydrosulfide of 0.6 mol, decompose Bunte salt；4) 2-6 hours are stood, up to crude product after layered shaping；5) step 4 gained crude product is put into rectifying still, carries out rectification under vacuum, 90 ~ 110 DEG C of bottom temperature of control collects 62 ~ 64 DEG C/100Pa of temperature, obtains Diallytrisin product.

Description

A kind of preparation method of Diallytrisin

Technical field:

Present invention relates particularly to a kind of preparation methods of Diallytrisin, belong to chemical technology field.

Background technique:

Diallytrisin be a kind of yellow liquid, have disgusting smell, 112~120 DEG C of boiling point (2133Pa) or 95~97 DEG C (667Pa) or 70 DEG C (133Pa), not soluble in water and ethyl alcohol is miscible in ether.Main application is Medicine intermediate, food additives, feed addictive.The preparation method of existing Diallytrisin be using S and Na2S by 2:1 synthesizes Na2S3, and then Na2S3 is reacted with allyl chloride by 1:2；Since the vulcanized sodium of synthesis is based on Na2S3 and to contain The mixture of Na2S, Na2S2, Na2S4 etc., crude product ingredient is more miscellaneous after processing, main peak content about 40%.

Summary of the invention:

In view of this, raw material is easy to get the present invention provides a kind of synthetic method is simple, reaction step is few, and finished product content is high Diallytrisin preparation method.

To achieve the above object, the technical solution adopted by the present invention are as follows:

A kind of preparation method of Diallytrisin is prepared by following raw material through special process: pure water 280 Part, 300 parts of the dodium thiosulfate of 1.2mol, 150 parts of sodium hydrosulfide of 92 parts of the chloropropene of 1.2mol, 0.6 mol.

A kind of preparation method of Diallytrisin, comprising the following steps:

1) sodium hydrosulfide for taking 50 parts of NaHS that 0.6 mol is made with 100 parts of water is spare；

2) 1000ml there-necked flask, 280 parts of pure water of addition, 300 parts of the dodium thiosulfate of 1.2mol, the chloropropene of 1.2mol are taken 92 parts, Bunte salt is made；

3) 30 ~ 50 DEG C of temperature control stir lower a dropping step 1) prepared by 150 parts of sodium hydrosulfide of 0.6 mol, decompose Bunte salt；

4) 2-6 hours are stood, 86 parts of crude product to obtain the final product after layered shaping, content 82.5%;

5) rectification under vacuum is carried out with 100ml three-necked flask, shunt head, 90 ~ 110 DEG C of bottom temperature of control collects temperature 62 ~ 64 DEG C/100Pa, obtain the Diallytrisin product of 66 parts of contents 92%.

The beneficial effects of the present invention are: synthetic method is simple, raw material is easy to get, and production cost is low, and reaction step is few, and finished product contains Amount is high, is suitble to large-scale production.

Specific embodiment:

To further elucidate this programme, the preferred embodiments of the invention are described combined with specific embodiments below, these Description is intended merely to further illustrate advantages of the present invention, rather than limiting to the claimed invention.

Embodiment 1

A kind of preparation method of Diallytrisin, comprising the following steps:

1) sodium hydrosulfide for taking NaHS 50g and 100g water that 0.6 mol is made is spare；

2) 1000ml there-necked flask is taken, pure water 280g, the chloropropene of the dodium thiosulfate 300g, 1.2mol of 1.2mol is added Bunte salt is made in 92g；

3) 40 ~ 50 DEG C of temperature control stir lower a dropping step 1) prepared by 0.6 mol sodium hydrosulfide 150g, decompose Bunte salt；

4) 5 hours are stood, up to crude product 86g, content 82.5% after layered shaping;

5) rectification under vacuum is carried out with 100ml three-necked flask, shunt head, 90 ~ 110 DEG C of bottom temperature of control collects temperature 62 ~ 64 DEG C/100Pa, obtain the Diallytrisin product of 66g content 92%.

Embodiment 2

A kind of preparation method of Diallytrisin, comprising the following steps:

1) sodium hydrosulfide for taking NaHS 50kg and 100kg water that 0.6 mol is made is spare；

2) pure water 280kg, the chloropropene 92kg of the dodium thiosulfate 300kg, 1.2mol of 1.2mol are added into reaction kettle, Bunte salt is made；

3) 45 ~ 50 DEG C of temperature control stir lower a dropping step 1) prepared by 0.6 mol sodium hydrosulfide 150kg, decompose Bunte salt；

4) 6 hours are stood, up to crude product 86kg, content 82.5% after layered shaping;

5) crude product 86kg obtained by step 4) is put into 100L rectifying still, progress rectification under vacuum, 90 ~ 110 DEG C of bottom temperature of control, 62 ~ 64 DEG C/100Pa of temperature is collected, the Diallytrisin product of 66kg content 92% is obtained.

The present invention is using allyl chloride and dodium thiosulfate quantitative reaction, controlled syntheses Bunte salt, then with quantitative NaHS Bunte salt is decomposed, what is obtained is relatively simple ideal product, therefore product yield and quality are higher.

The above is only the preferred embodiment of the present invention, above-mentioned preferred embodiment is not construed as limitation of the present invention, Protection scope of the present invention should be defined by the scope defined by the claims..Those skilled in the art are come It says, without departing from the spirit and scope of the present invention, several improvements and modifications can also be made also and should be regarded as protection of the invention Range.

Claims

1. a kind of preparation method of Diallytrisin, it is characterised in that: be prepared from the following materials: 280 parts of pure water, 300 parts of the dodium thiosulfate of 1.2mol, 150 parts of sodium hydrosulfide of 92 parts of the chloropropene of 1.2mol, 0.6 mol, including it is following Step:

2) it takes 1000ml there-necked flask, is added 280 parts of pure water, 300 parts of the dodium thiosulfate of 1.2mol, 92 parts of the chloropropene of 1.2mol, Bunte salt is made；

4) 2-6 hours are stood, up to crude product after layered shaping；

5) step 4 gained crude product is put into rectifying still, carries out rectification under vacuum, 90 ~ 110 DEG C of bottom temperature of control collects temperature 62 ~ 64 DEG C/100Pa, obtain Diallytrisin product.