ethylenebis(oxyethylene) dihexanoate synthesis
- Product Name:ethylenebis(oxyethylene) dihexanoate
- CAS Number:25176-75-4
- Molecular formula:C18H34O6
- Molecular Weight:346.46
Yield:25176-75-4 96%
Reaction Conditions:
with potassium carbonate at 155; under 750.075 Torr; for 6 h;
Steps:
2 Example 2
Example 2
This embodiment serves to illustrate the present invention prepartion method of triethylene glycol di-n-hexanoate
In a 100ml round-bottomed flask with condenser, liquid separator and stirrer was added 15.07g (0.1mol) triethylene glycol (determined by gas chromatography analysis of chromatographic purity 99.2%),52.58g (0.4mol) hexanoic acid methyl ester, 2.78g (0.02mol) of anhydrous potassium carbonate, contacting round bottom flask in an oil bath and was heated to 155°C, in 0.1MPa reaction, during reaction, simultaneously go through distillation to separate and remove the generated distilled alcohol. After 6h of reaction, toluene was added to the round-bottomed flask. Before and after it was added a total of 6 times , was added in two adjacent intervals of 2 hours, each time adding 12mL, for each time toluene is added, it was reacted for 1.5 hours at 150°C and at the same time toluene and azeotropes of the round-bottomed flask was distilled off . After the reaction mixture was cooled for approximately 30 minutes, the next toluene was added. After completion of reaction, the round-bottomed flask was cooled down and filtered to remove anhydrous potassium carbonate. Again, vacuum distill the filtrate at 667Pa and 76°C to remove unreacted hexanoic acid methyl ester and other impurities. And then under 667 Pa at 44°C, vacuum distillation to remove the unreacted hexanoic acid methyl ester and other impurities, Obtaining triethylene glycol di-n-hexanoate, yield 96%, by gas chromatography spectrum-mass spectrometry (GC-MS) analysis, the purity of 97.4%. The results are shown in Table 1.
References:
CN104045555,2016,B Location in patent:Paragraph 0039; 0040; 0041
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