HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → (4-Bromo-naphthalen-1-yl)-oxo-acetic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 1-Bromonaphthalene | HCID 7001 | — |
| Reactant | Methyl chloroglyoxylate | HCID 79846 | — |
| Reactant | Aluminum(III) Chloride | HCID 6451240 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (4-Bromo-naphthalen-1-yl)-oxo-acetic acid methyl ester | HCID 59379801 | 37% |
Reaction Steps
To a suspension of AlCl3 (3.20 g, 24 mmol) in 100 mL DCM at 0° C., methylchloroglyoxylate (2.2 mL, 24 mmol) was added. The resulting solution was stirred for 5 min., after which 1-bromo-naphthalene (5 g, 24 mmol) was added. After stirring for 2 hrs at room temperature, water was added and the phases were separated, after which the organic layer was washed with water and dried over MgSO4. The residue obtained after evaporation of the organic solvent was purified by column chromatography (0-30% EtOAc/Hex), to afford 2.6 g of the target compound. 1H NMR (CDCl3): 8.92 (1H, d, J=9.3 Hz, H-arom); 8.31 (1H, d, J=9.3 Hz, H-arom); 7.82 (1H, d, J=8.8 Hz, H-arom); 7.72 (1H, d, J=8.8 Hz, H-arom); 7.57-7.68 (2H, m, H-arom); 3.94 (3H, s, OMe).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07897599B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-04606159128b40cf95896d331dc8e72a |
| Source note | uspto-grants-2011_03 |