HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 13708900, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | HCID 13708886 | HCID 13708886 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 13708900 | HCID 13708900 | 110.6% |
Reaction Steps
Fifty milliliters of an ether solution of 30.1 g of ethyl 4,4,4-trifluoro-3-tetrahydropyranyloxybutyrate (1) were added dropwise to an ether suspension of 4.2 g of lithium aluminum hydride over a period of 1.5 hours. The mixture was further refluxed for 30 minutes, and a mixed solution of 8 g of water and 50 ml of tetrahydrofuran was added dropwise under ice cooling. The solid was separated by filtration and extracted with ether. After drying, the ether was evaporated to obtain 28.1 g of 4,4,4-trifluoro-3-tetrahydropyranyloxybutyl alcohol (2) in a purity of 65%. Since the compound (2) was relatively unstable to heat and acid, said compound was only dried in pyridine with a molecular sieve 4A and used in the subsequent step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05264150 |
| Source dataset | uspto-grants-1993_11 |
| ORD ID | ord-2becc26ecd684d9d90275894f7d79676 |
| Source note | uspto-grants-1993_11 |