4-METHOXY-3-METHYLACETOPHENONE

4-METHOXY-3-METHYLACETOPHENONE Property

Melting point:

26-26.5 °C

Boiling point:

251.67°C (rough estimate)

Density 

1.0326 (rough estimate)

refractive index 

1.5460 (estimate)

storage temp. 

Sealed in dry,Room Temperature

solubility 

Chloroform (Slightly), Methanol (Slightly)

form 

Oil

color 

Dark Yellow

Safety

HS Code 

2914500090

Hazard and Precautionary Statements (GHS)

Symbol(GHS)

Signal word

Warning

Hazard statements

H315Causes skin irritation

H319Causes serious eye irritation

H335May cause respiratory irritation

Precautionary statements

P264Wash hands thoroughly after handling.

P264Wash skin thouroughly after handling.

P280Wear protective gloves/protective clothing/eye protection/face protection.

P302+P352IF ON SKIN: wash with plenty of soap and water.

P305+P351+P338IF IN EYES: Rinse cautiously with water for several minutes. Remove contact lenses, if present and easy to do. Continuerinsing.

P321Specific treatment (see … on this label).

P332+P313IF SKIN irritation occurs: Get medical advice/attention.

P362Take off contaminated clothing and wash before reuse.

4-METHOXY-3-METHYLACETOPHENONE Chemical Properties,Usage,Production

Preparation

Preparation by reaction of acetic anhydride with 2-methylanisole in the presence of lithium perchlorate at 60° for 1.5 h (99%).

Synthesis

1. Dimethyl sulfate (17.50 mL, 183 mmol) was slowly added to a stirred suspension of 1-(4-hydroxy-3-methylphenyl)ethanone (25 g, 166 mmol) and potassium carbonate (28.8 g, 208 mmol) in acetone (277 mL). The reaction was carried out at room temperature. 2. The reaction mixture was heated to reflux and stirred continuously overnight. 3. Upon completion of the reaction, it was cooled to room temperature, the solids were separated by filtration, and the solids were washed with acetone. 4. The filtrate was concentrated under vacuum to remove the solvent. 5. The concentrated organic residue was dissolved in ethyl acetate (EtOAc) and the organic layer was washed with water. 6. The organic layer was separated, dried with anhydrous magnesium sulfate (MgSO?), filtered, and the solvent was evaporated under vacuum to give 1-(4-methoxy-3-methylphenyl)ethanone (28.7 g) as a yellow oil. The product did not require further purification and could be used directly in the next reaction.

References

[1] Patent: WO2015/12708, 2015, A1. Location in patent: Page/Page column 14; 15
[2] Patent: CN107337596, 2017, A. Location in patent: Paragraph 0039; 0040; 0044; 0045