1,3-BENZENEDIMETHANETHIOL synthesis
- Product Name:1,3-BENZENEDIMETHANETHIOL
- CAS Number:41563-69-3
- Molecular formula:C8H10S2
- Molecular Weight:170.29
626-16-4
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41563-69-3
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Yield:41563-69-3 55 g
Reaction Conditions:
Stage #1: 3-(chloromethyl)benzyl chloridewith thiourea in water; for 2.5 h;Inert atmosphere;Reflux;
Stage #2: with water;sodium hydroxide at 40 - 70; for 2 h;Inert atmosphere;Temperature;
Steps:
1 Example 1
Example 1
Synthesis 1 of m-Xylylene Dithiol (Compound a-1) Containing a Small Amount of the Compound (b)
In a 1 L four-neck reaction flask equipped with a stirring machine, a reflux cooling tube, a nitrogen gas purge tube and a thermometer, 74.1 g of m-xylylene dichloride, 67.2 g of thiourea and 270 g of water were mixed together, and the mixture was heated to reflux for 2.5 hours.
The mixture was cooled to room temperature, and then 134.1 g of 50% aqueous solution of sodium hydroxide was added thereto under nitrogen atmosphere, and the mixture was hydrolyzed at 70° C. to 40° C. for 2 hours.
Next, the reaction solution was cooled to 40° C., hydrochloric acid was added thereto until pH became 2, and subsequently the mixture was stirred for 30 minutes to carry out neutralization.
After the reaction was completed, extraction was carried out with 360 mL of toluene, and then toluene and a slight amount of water were removed under reduced pressure with heating.
After that, a polythiol composition containing m-xylylene dithiol obtained was purified by distillation, and then washed with water.
The pressure was reduced with heating to remove water, and then filtration was carried out, thereby obtaining 55.0 g of a polythiol composition. In this polythiol composition, the content percentage of the corresponding compound (b) was 0.05% by mass. Further, the content percentage of m-xylylene dithiol was 99.6% by mass.
References:
US2017/247322,2017,A1 Location in patent:Paragraph 0034-0035
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