HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 4-[[6-[3,4-Dimethoxy-5-(1-methylethyl)phenyl)-6-oxohexyl]oxy]-2-hydroxy-3-propylbenzoic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Methyl 2,4-dihydroxy-3-propylbenzoate | HCID 13019281 | — |
| Reactant | 6-Bromo-1-[3,4-dimethoxy-5-(1-methylethyl)phenyl]-1-hexanone | HCID 14986400 | — |
| Solvent | Acetone | HCID 180 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 4-[[6-[3,4-Dimethoxy-5-(1-methylethyl)phenyl)-6-oxohexyl]oxy]-2-hydroxy-3-propylbenzoic acid methyl ester | HCID 14986415 | 98.9% |
Reaction Steps
A mixture of 6.0 g (0.017 mol) of 6-bromo-1-[3,4-dimethoxy-5-(1-methylethyl)phenyl]-1-hexanone, 3.39 g (0.016 mol) of 2,4-dihydroxy-3-propylbenzoic acid methyl ester and 7.0 g (0.051 mol) of potassium carbonate in 120 mL of acetone and 12 mL of DMF was stirred at reflux for 19 hours. After workup as in Example 16, the crude product was purified by HPLC using 16% ethyl acetate-hexane to give 7.7 g (98% yield) of 4-[[6-[3,4-dimethoxy-5-(1-methylethyl)phenyl)-6-oxohexyl]oxy]-2-hydroxy-3-propylbenzoic acid methyl ester as an oil. The nmr spectrum was consistent with the structure.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05191108 |
| Source dataset | uspto-grants-1993_03 |
| ORD ID | ord-24774a4368774572975421f85b4dab6b |
| Source note | uspto-grants-1993_03 |