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ChemicalBook CAS DataBase List Ethyl 4-acetylbutyrate

Ethyl 4-acetylbutyrate synthesis

14synthesis methods
30ml of acetone and 11.5mmol of tetrahydropyrrole were added to a dry three-necked flask equipped with a thermometer and reflux condenser, and then slowly add 50mmol of ethyl acrylate dropwise at 60°C for 10h. After the reaction, the reaction solution is at 60°C Distill the remaining unreacted acetone and acidify with dilute hydrochloric acid to adjust the pH to 4. Add ethyl acetate for extraction, collect the organic layer, and perform preliminary vacuum distillation at 0.1MPa vacuum and 45°C to distill off the low-boiling solvent, followed by 3- Collect 70-80°C fractions under a vacuum of 7mmHg to prepare Ethyl 4-acetylbutyrate.
Ethyl 4-acetylbutyrate
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Yield:13984-57-1 34%

Reaction Conditions:

with Potassium phosphate, dibasic at 60; for 6 h;Michael Addition;

Steps:

2 Example 2

Put 58g (1mol) acetone and 1.74g (10mmol) K2HPO4 in a dry three-necked flask equipped with a thermometer and a reflux condenser, then slowly add 10g (0.1mol) ethyl acrylate (3h dripping), at 60 ° C The reaction was carried out for 3 hours; after the reaction, the remaining unreacted acetone and methyl acrylate were distilled off from the reaction solution at 80° C. to obtain 9.22 g of ethyl 5-oxohexanoate with a yield of 34% and a selectivity of 90%.

References:

CN114516796,2022,A Location in patent:Paragraph 0031-0032

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