HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Fluorophenol → (S)-4-[(4-fluorophenoxy)methyl]-2,2-dimethyl-1,3-dioxolane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Fluorophenol | HCID 9732 | — |
| Reactant | Sodium | HCID 5360545 | — |
| Reactant | Methanesulfonic acid [(R)-2,2-dimethyl-[1,3]dioxolan-4-yl]methyl ester | HCID 15570842 | — |
| Solvent | 2-Methoxyethanol | HCID 8019 | — |
| Product | (S)-4-[(4-fluorophenoxy)methyl]-2,2-dimethyl-1,3-dioxolane | HCID 15725175 | 97.3% |
Reaction Steps
To a stirred solution of 2.7 parts of sodium in 50 parts of 2-methoxyethanol were added 13.2 parts of 4-fluorophenol. The whole was stirred for 15 minutes. A solution of 24.8 parts of (-)-(R)-2,2-dimethyl-1,3-dioxolane-4-methanol methanesulfonate (ester) in 70 parts of 2-methoxyethanol was added dropwise quickly. Stirring was continued for 1.5 hours at reflux temperature. After cooling, the mixture was poured into ice water. The product was extracted with methylbenzene. The extract was dried, filtered and evaporated, yielding 26 parts (97.3%) of (S)-4-[(4-fluorophenoxy)methyl]-2,2-dimethyl-1,3-dioxolane as a residue (145).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04861785 |
| Source dataset | uspto-grants-1989_08 |
| ORD ID | ord-0c0ef33e98014719bef3c2210b2752d2 |
| Source note | uspto-grants-1989_08 |