HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfoxide → (+/-)-7-(4-Fluorophenoxy)-6-(2-methoxyethoxymethoxy)-heptan-1-al
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfoxide | HCID 679 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | (+/-)-7-(4-Fluorophenoxy)-6-(2-methoxyethoxymethoxy)heptan-1-ol | HCID 18533434 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (+/-)-7-(4-Fluorophenoxy)-6-(2-methoxyethoxymethoxy)-heptan-1-al | HCID 18533431 | — |
Reaction Conditions
| Temperature | -78 °C |
|---|
Reaction Steps
Oxalyl chloride (2.9 ml, 33.6 mmol) is added to 25 ml of methylene chloride and cooled to −78° C. Dry dimethyl sulfoxide (4.7 ml, 67.2 mmol) is then added and the reaction is stirred at −78° C. After 45 minutes, (±)-7-(4-fluorophenoxy)-6-(2-methoxyethoxymethoxy)-heptan-1-ol 44 (3.7 g, 11.2 mmol) dissolved in CH2Cl2 is added and the reaction is stirred at −78° C. After 1 hour, the reaction is quenched with 15.7 ml of triethylamine and diluted with CH2Cl2. The reaction mixture is then washed with water, brine dried (Na2SO4) and concentrated. The crude product is purified on silica gel (ethyl acetate:hexane 1:9) to give (±)-7-(4-fluorophenoxy)-6-(2-methoxyethoxymethoxy)-heptan-1-al 45, 3.3 g, 89%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06433197B1 |
| Source dataset | uspto-grants-2002_08 |
| ORD ID | ord-06dd8d0f89564a0ca4291e74fe04f43e |
| Source note | uspto-grants-2002_08 |