HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 9856261, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 4,5-Dichloro-4,5-difluoro-2,2-bis(trifluoromethyl)-1,3-dioxolane | HCID 162919 | — |
| Reactant | HCID 21189139 | HCID 21189139 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 9856261 | HCID 9856261 | 69.1% |
Reaction Steps
In a round-bottomed flask was charged lithium aluminum hydride (3.8 g, 0.1 mole) in tetrahydrofuran (75 mL) and the contents was cooled in an ice-water bath at 0° to 5° C. 4,5-Dichloro-4,5-difluoro-2,2-bis(trifluoromethyl)-1,3-dioxolane (31.5 g, 0.1 mole) was added slowly. After the addition was complete, the reaction mixture was stirred at room temperature for 30 minutes. The resulting mixture was neutralized with 4.8N HCl (50 mL), then poured into 300 mL of ice-water. The bottom layer was separated and washed twice with cold water (200 mL). Distillation gave the saturated product 4,5-difluoro-2,2-bis(trifluoromethyl)-1,3-dioxolane (17 g, 69% yield) instead of the unsaturated dioxole product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04908461 |
| Source dataset | uspto-grants-1990_03 |
| ORD ID | ord-8c820ee835b64b77b9efe3c6f960c43c |
| Source note | uspto-grants-1990_03 |