HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl 2-(1,4-dioxaspiro[4.5]decan-8-yl)acetate → 2-(1,4-Dioxaspiro(4.5)decan-8-yl)ethan-1-ol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl 2-(1,4-dioxaspiro[4.5]decan-8-yl)acetate | HCID 15700391 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2-(1,4-Dioxaspiro(4.5)decan-8-yl)ethan-1-ol | HCID 11805458 | 97.9% |
Reaction Steps
To a mixture of lithium aluminum hydride (42.5 g, 1.12 mol) in THF (1200 mL) is carefully added crude 8-ethoxycarbonylmethyl-1,4-dioxaspiro[4.5]decane (174.7 g) in THF solution (640 mL) at 0° C. under argon atmosphere. After stirring for 10 min at ambient temperature, Na2SO4-10H2O (360.9 g) is added at 0° C., and the mixture is stirred for additional 3 hours. Insoluble matter is filtered and washed with EtOAc, and the filtrate is concentrated in vacuo to afford crude 2-(1,4-dioxaspiro[4.5]dec-8-yl)ethanol (139.5 g). The crude product is used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08410275B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-d6232f01dcb74fb3a60fe58f0cf2c179 |
| Source note | uspto-grants-2013_04 |