HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetone → 4-[2-Methyl-4-(2-methyl-benzyloxy)-phenyl]-but-3-en-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetone | HCID 180 | — |
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 2-Methyl-4-(2-methyl-benzyloxy)-benzaldehyde | HCID 86602460 | — |
| Solvent | Water | HCID 962 | — |
| Product | 4-[2-Methyl-4-(2-methyl-benzyloxy)-phenyl]-but-3-en-2-one | HCID 68674218 | 63% |
Reaction Steps
2N NaOH(aq) (0.6 mL) was added to a solution of 31.3 (100 mg, 0.42 mmol) in acetone (1 mL). The reaction was stirred at room temperature overnight and then taken up in water. The aqueous solution was acidified with 1N HCl(aq) (1.5 mL) and extracted with ethyl acetate. The organic extracts were washed with brine, dried (Na2SO4), and concentrated in vacuo. The resultant residue was purified via radial chromatography (20% ethyl acetate in hexanes) to yield 74 mg (63%) of 4-[2-Methyl-4-(2-methyl-benzyloxy)-phenyl]-but-3-en-2-one (31.4). LC/MSD m/e: 281.4 (M+H); 1H NMR (400 MHz) (acetone-d6) δ 7.83 (1H, d, J=16), 7.70 (1H, m), 7.46 (1H, m), 7.25 (3H, m), 6.96 (2H, m), 6.63 (1H, d, J=16 Hz).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07816367B2 |
| Source dataset | uspto-grants-2010_10 |
| ORD ID | ord-19a26eb2fd394e36a454915bbff02918 |
| Source note | uspto-grants-2010_10 |