Triethyl 1,1,2-ethanetricarboxylate synthesis
- Product Name:Triethyl 1,1,2-ethanetricarboxylate
- CAS Number:7459-46-3
- Molecular formula:C11H18O6
- Molecular Weight:246.26
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Step a): Sodium metal (23 g, 1 mole) was slowly added to anhydrous ethanol (500 mL) under stirring conditions until completely dissolved. Subsequently, diethyl malonate (160 g, 1 mole) was added dropwise over 30 min. After cooling the reaction mixture to 15°C, ethyl chloroacetate (117 g, 0.095 mol) was added dropwise over the same time. After the dropwise addition, the reaction mixture was refluxed for 6 hours. After completion of the reaction, the mixture was poured into 2 liters of water and the organic phase was extracted with dichloromethane (500 mL each time, three times). The organic extracts were combined, dried with anhydrous sodium sulfate, filtered and the solvent was evaporated to give an oily crude product. Finally, purification by vacuum distillation afforded triethyl ethyl-1,1,2-tricarboxylate (220 g, 89% yield).
Yield:7459-46-3 93.8%
Reaction Conditions:
with tetrabutylammonium bromide;anhydrous sodium carbonate;sodium iodide in toluene at 20 - 120;Solvent;Reagent/catalyst;
Steps:
4 Example 4
In 1000ml reaction flask installed with a stirrer, athermometer, a pressure-equalizing dropping funnel, a glass trap and condenser,At room temperature, the solvent toluene 500ml, openstirring, diethyl malonate100g, acid binding agent sodium bicarbonate 105g, sodium iodide catalyst8. 5g, phase transfer catalyst is tetrabutylammonium bromide 8. 0g, feedingafter the completion of the slow heating, the temperature raise to 20 ° C ~ 115° C, the dropwise addition of ethyl bromoacetate 104. 5g, dropping time control in 1.0 hours,the reaction incubated 1.5 hours, slowly warming to 20 ~ 120 ° C (TC thermalreaction, as the reaction to produce water, carried through the watershed trap,reflux heat for 8 to 12 hours until dry produce inside the trap during thereaction system color transparent white; sampling analysis, after passing thecontrol, cooling down to about 10 ° C, and acetic acid was slowly addeddropwise, regulating ΡΗ = 7, suction filtered, the inorganic salt was filteredoff, the filtrate was collected. the inorganic salt was washed with 50ml X 2with hot toluene, The filtrate was collected and the combined filtrate underreduced pressure solvent removal under reduced pressure to end off the solventcontrol the degree of vacuum -0.098Mpa, vacuum distillation final temperatureof about 120 ~ 130 ° C, vacuum degassing solvent condenser end when there is no condensed liquid stream to give a colorless or pale yellow liquid product 145.1g, the yield is about 93.8%.
References:
CN105566111,2016,A Location in patent:Paragraph 0031
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