5-METHOXY-3-OXOVALERIC ACID METHYL ESTER

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5-METHOXY-3-OXOVALERIC ACID METHYL ESTER Basic information
Product Name:5-METHOXY-3-OXOVALERIC ACID METHYL ESTER
Synonyms:5-METHOXY-3-OXOVALERIC ACID METHYL ESTER;3-KETO-5-METHOXYVALERIC ACID METHYL ESTER;NAZAROV REAGENT;METHYL 5-METHOXY-3-OXOALERATE;5-Methoxy-3-oxopentanoic acid methyl ester;3-Keto-5-methoxyvaleric Acid Methyl Ester 5-Methoxy-3-oxovaleric Acid Methyl Ester Methyl 3-Keto-5-methoxyvalerate;METHYL 5-METHOXY-3-OXOPENTANOATE;METHYL 5-METHOXY-3-OXOVALERATE
CAS:62462-05-9
MF:C7H12O4
MW:160.17
EINECS:263-553-9
Product Categories:
Mol File:62462-05-9.mol
5-METHOXY-3-OXOVALERIC ACID METHYL ESTER Structure
5-METHOXY-3-OXOVALERIC ACID METHYL ESTER Chemical Properties
Boiling point 56-57 °C/0.1 mmHg (lit.)
density 1.10 g/mL at 20 °C (lit.)
refractive index n20/D 1.44
Fp 104 °C
storage temp. Storage temp. 2-8°C
pka10.38±0.46(Predicted)
form clear liquid
color Colorless to Almost colorless
BRN 2042099
InChI1S/C7H12O4/c1-10-4-3-6(8)5-7(9)11-2/h3-5H2,1-2H3
InChIKeyOPURNNHYTATPKM-UHFFFAOYSA-N
SMILESCOCCC(=O)CC(=O)OC
LogP0.497 (est)
Safety Information
WGK Germany 3
HS Code 2918999090
Storage Class10 - Combustible liquids
MSDS Information
ProviderLanguage
SigmaAldrich English
5-METHOXY-3-OXOVALERIC ACID METHYL ESTER Usage And Synthesis
Uses5-METHOXY-3-OXOVALERIC ACID METHYL ESTER is used as a precursor to the annulating agent and Nazarov's reagent.[1] It can function as an annulating agent under acidic reaction conditions.[2]
Synthesis Reference(s)Synthesis, p. 622, 1979 DOI: 10.1055/s-1979-28786
Synthesis
3-METHOXYPROPIONIC ACID

2544-06-1

Potassium 3-methoxy-3-oxopropanoate

38330-80-2

5-METHOXY-3-OXOVALERIC ACID METHYL ESTER

62462-05-9

1. 3-Methoxypropionic acid (1.81 mL, 19.2 mmol) was suspended in anhydrous acetonitrile (80 mL) and stirred. 2. Methyl 5-methoxy-3-oxopentanoate (3.24 g, 20.0 mmol) was added in one portion and the reaction mixture was stirred at room temperature for 1.5 h. 3. A powdered mixture of magnesium chloride (1.57 g, 16.5 mmol) and potassium methyl malonate (4.5 g, 28.8 mmol) was added in one portion (note that CO2 gas was produced during the reaction). 4. The reaction mixture continued to be stirred at room temperature. 5. MgCl2 (1.57 g, 16.5 mmol) and potassium malonate monohydrate (4.5 g, 28.8 mmol) in a powdered mixture (note that CO2 gas is produced during the reaction). 4. Continue to stir the reaction mixture at room temperature. 5. Vacuum remove the volatiles, then add 2M hydrochloric acid (105 mL). 6. Stir the solution for 1 hour at room temperature, and then extract it with dichloromethane (3 x 100 mL). 7. Combine the organic phases, dry them with MgSO4, filter, and remove the solvents in vacuum. 8. dried, filtered and the solvent was removed in vacuum to afford the target product methyl 5-methoxy-3-oxovalerate (2.69 g, 87% yield).

References[1] Patent: WO2016/83816, 2016, A1. Location in patent: Page/Page column 46
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