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5-Methyl-2-hexenoic acid synthesis

6synthesis methods
-

Yield:41653-96-7 98%

Reaction Conditions:

with trimethyl-(2-hydroxyethyl)ammonium chloride;carbamide at 80;

Steps:

1 Example 1 Synthesis of 5-methyl-2-hexenoic acid:

In a dry three-necked flask, 1.4 g (1 mol) of choline chloride and 1.2 g (2 mol) of urea were added. The temperature was raised to 80 ° C, and the mixture was magnetically stirred to obtain a colorless transparent liquid, that is, the eutectic solvent DES1 (choline chloride- Urea) and cooled to room temperature; then 0.500 g (1 mol) of isovaleraldehyde and 0.725 g (1.2 mol) of malonic acid were added, the temperature was raised to 80 ° C., and the reaction was stirred, and the reaction was monitored by TLC until the reaction was complete. After the reaction, it was cooled to room temperature, added a small amount of water, extracted with ethyl acetate, the organic layer was washed with water, dried, and the solvent was distilled off to obtain 5-methyl-2-hexenoic acid, a yellow liquid, with a yield of 98. %. Water phase is evaporated to recover DES, which can be reused.

References:

CN110803994,2020,A Location in patent:Paragraph 0022; 0023-0025

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