HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → 1,4-Dioxaspiro[4.5]decane-8-carboxylic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | Ethyl 1,4-dioxaspiro(4.5)decane-8-carboxylate | HCID 10488810 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 1,4-Dioxaspiro[4.5]decane-8-carboxylic acid | HCID 11745334 | — |
Reaction Steps
3.0 g (14 mmol) of the ethyl ester precursor, ethyl 1,4-dioxaspiro[4.5]decane-8-carboxylate, were dissolved in 5 ml of methanol and admixed at RT slowly with 28 ml (2 eq.) of 1 M LiOH solution. The mixture was stirred overnight; HPLC-MS indicated complete reaction. Methanol was distilled off under reduced pressure and the residue was acidified cautiously with 1 ml of HCl such that no acid excess was present. The mixture was extracted with ethyl acetate, and the ethyl acetate phase was dried over sodium sulfate and then concentrated by evaporation under reduced pressure. Yield: 2.25 g, 86% of theory.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08609681B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-8227287cd1af4969bc86b4ecd06e84bc |
| Source note | uspto-grants-2013_12 |