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Method for catalyzing and synthesizing ditert-butyl disulphide by trichlorine molybdenum monoxide compounded by methyl-sulfoxide

A technology of di-tert-butyl disulfide and molybdenum trichloride is applied in the directions of organic compound/hydride/coordination complex catalysts, chemical instruments and methods, physical/chemical process catalysts, etc. Butyl disulfide, difficult to industrialize production, large steric hindrance and other problems, to achieve the effect of small dosage, beneficial to industrial production and high conversion rate

Active Publication Date: 2009-12-23
ZHENGZHOU UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many preparation methods of di-tert-butyl disulfide, which can be prepared mainly from two raw materials, one is the method of using tert-butyl halide (tert-butyl chloride or tert-butyl bromide) as raw material, and it is prepared by reacting with sodium disulfide Disulfide, but when using this method to prepare di-tert-butyl disulfide, because the tert-butyl carbon in the tert-butyl halide structure is a quaternary carbon atom, the steric hindrance is large, and it is difficult to obtain di-tert-butyl disulfide smoothly. Ether, therefore, the method for preparing di-tert-butyl disulfide with tert-butyl halide is difficult to industrialized production
But the disadvantage of this method is that the price of NCS is high, a large amount of lye is needed for post-treatment, and the yield of reaction is also low (80%)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Put 14.4g (0.1mol) of molybdenum trioxide and 14.5ml (0.2mol) of thionyl chloride in a 150ml three-necked flask, react at reflux temperature for 4h, and cool to room temperature. Mix 3.3ml (0.05mol) of absolute ethanol with 14.1ml (0.2mol) of DMSO, and slowly drop it into the reaction system drop by drop under cooling in an ice bath to obtain a green solid, which is washed with cold absolute ethanol to obtain a green The powdery solid was vacuum-dried to obtain 30.90 g of the product, with a yield of 82.5%. m.p.135~136℃, 1 HNMR (400MHZ, d 6 -DMSO) δ: 2.54 (s, 18H).

Embodiment 2

[0019] Put 14.4g (0.1mol) of molybdenum trioxide and 18.1ml (0.25mol) of thionyl chloride in a 150ml three-neck flask, react at reflux temperature for 6h, and cool to room temperature. Mix 3.3ml (0.05mol) of absolute ethanol with 14.1ml (0.2mol) of DMSO, and slowly drop it into the reaction system drop by drop under cooling in an ice bath to obtain a green solid, which is washed with cold absolute ethanol to obtain a green The powdery solid was vacuum-dried to obtain 32.20 g of the product, with a yield of 90.9%. Melting point and spectral data are the same as above.

Embodiment 3

[0021] Put 7.2g (0.05mol) of molybdenum trioxide and 10.9ml (0.15mol) of thionyl chloride in a 150ml three-neck flask, react at reflux temperature for 2h, and cool to room temperature. Mix 14.5ml (0.25mol) of absolute ethanol with 7.05ml (0.1mol) of DMSO, and slowly drop it into the reaction system drop by drop under cooling in an ice bath to obtain a green solid, which is washed with cold absolute ethanol to obtain a green The powdery solid was vacuum-dried to obtain 15.16 g of the product, with a yield of 80.9%. Melting point and spectral data are the same as above.

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Abstract

The invention discloses a synthesis method for ditert-butyl disulphide, relating to the method for synthesizing ditert-butyl disulphide by using trichlorine molybdenum monoxide catalyst. The method is as follows: tert-butyl thiols and MoOCl3 (DMSO)2 obtained by the invention are blended with DMSO, is heated and reacts; reaction liquid is poured into alkali liquor, sets aside and layered to obtain ditert-butyl disulphide. MoOCl3 (DMSO)2 compounded by the method has excellent catalyzing effect, few dosage, good reaction selectivity, and high conversion rate in the process of preparing ditert-butyl disulphide by catalyzing tert-butyl thiols; simultaneously, the yield and purity of the ditert-butyl disulphide are high; the after-treatment is simple and convenient; and the ditert-butyl disulphide can be applied to industrialization production.

Description

technical field [0001] The invention relates to a synthesis method of di-tert-butyl disulfide, in particular to a method for catalytically synthesizing di-tert-butyl disulfide by using molybdenum trichloride monoxide catalyst complexed with dimethyl sulfoxide, belonging to the technical field of organic synthesis. Background technique [0002] Disulfide has important application value in the fields of food science, biochemistry and flavor chemistry, among which di-tert-butyl disulfide is an important raw material for preparing fine chemical intermediates such as tert-butylsulfinyl chloride. There are many preparation methods of di-tert-butyl disulfide, which can be prepared mainly from two raw materials, one is the method of using tert-butyl halide (tert-butyl chloride or tert-butyl bromide) as raw material, and it is prepared by reacting with sodium disulfide Disulfide, but when using this method to prepare di-tert-butyl disulfide, because the tert-butyl carbon in the tert-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C321/14C07C319/24B01J31/22
Inventor 李雯章亚东樊璐露胡国勤赵文恩周游赵松芳兀吉康
Owner ZHENGZHOU UNIV