Tetraethyl orthocarbonate synthesis
- Product Name:Tetraethyl orthocarbonate
- CAS Number:78-09-1
- Molecular formula:C9H20O4
- Molecular Weight:192.25
Yield:78-09-1 91%
Reaction Conditions:
with sodium ethanolate at 65 - 70; for 3 h;Large scale;Temperature;
Steps:
1 Example 1
(1) Put 320 kg of sodium ethoxide and 1280 kg of absolute ethanol into a clean, dry 2000L reactor;(2) The control temperature is between 65°C and 70°C.Trichloronitromethane (97 kg) was added dropwise.After the addition, the reaction was continued for 3 hours, and 900 kg of absolute ethanol was recovered by atmospheric distillation.(3) 1600 kg of water was added to dissolve all the residue, and 1280 kg of n-heptane was added for extraction;(4) The organic phase enters the rectification tower, and 0.05 kg of sodium ethoxide is added. The normal pressure control reflux ratio is 1 to 2, and the normal pressure is 1024 kg of n-heptane.(5) The reflux ratio was controlled to be 3 to 5, and the product was rectified under the pressure of -0.098 MPa to produce tetraethylorthocarbonate. The total product was: 104 kg, purity 99.7%, single impurity <0.1%, yield 91%.
References:
CN107573223,2018,A Location in patent:Paragraph 0023-0028; 0029-0034; 0035-0040; 0041-0046
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