HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 18624471, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Iodine chloride | HCID 24640 | — |
| Reactant | Ethyl 2-ethoxy-3-(4-hydroxyphenyl)propanoate | HCID 11791243 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Product | HCID 18624471 | HCID 18624471 | 98.13% |
Reaction Steps
To stirred solution of racemic ethyl 2-ethoxy-3-(4-hydroxyphenyl)propionate of the formula (13a) (20 g) obtained according to the procedure described in step (v) above and dimineralised water (100 ml), ICl (13.6 g, 4.4 ml) in HCl (80 ml) was added dropwise at room temperature for 30 min. The reaction mixture was heated to 75° C. to 80° C. for 20 h. The progress of the reaction was monitored by TLC. After completion of the reaction, toluene (200 ml) was added to the reaction mixture and extracted with dimineralised water. Organic extracts were concentrated to yield the crude compound. The crude compound was purified by column chromatography using 3% ethyl acetate in pet. ether to yield the title compound (10.3 g, 98.13%)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06531596B1 |
| Source dataset | uspto-grants-2003_03 |
| ORD ID | ord-9d410289240247718b349103c773b1d6 |
| Source note | uspto-grants-2003_03 |