HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → HCID 23159322, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | Propanoic acid, 2-bromo-2-methyl-, ethyl ester | HCID 11745 | — |
| Reactant | 3,5-Dimethyl-4-hydroxybenzaldehyde | HCID 75222 | — |
| Solvent | 3-Methyl-2-butanone | HCID 11251 | — |
| Product | HCID 23159322 | HCID 23159322 | 90% |
Reaction Steps
A solution of 3,5-Dimethyl-4-hydroxybenzaldehyde (20 g, 0.133 mol) in 3-Methyl-2-butanone (400 mL) was treated with Cs2CO3 (86.9 g, 2 eq.) and Ethyl-2-bromoisobutyrate (39.2 L, 2 eq.). The resulting mixture was stirred at reflux for 36 hours. After cooling to rt the reaction mixture was filtered off. The cake was washed with ethyl acetate. The filtrate was evaporated off and the residue was diluted with ethyl acetate (1 L), washed with water (500 mL) and then with NaOH 1N (500 mL). The organic layer was drying over Na2SO4 and filtration evaporation gave the title compound (31.8 g, 0.12 mol) as a brown oil in a 90% yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07241793B2 |
| Source dataset | uspto-grants-2007_07 |
| ORD ID | ord-82b76abc90584f3aa4f8a79468151253 |
| Source note | uspto-grants-2007_07 |