HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium hydroxide, monohydrate → HCID 10273808, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 69683369 | HCID 69683369 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 10273808 | HCID 10273808 | 82.2% |
Reaction Steps
The ester (1 g), dissolved in 20 ml THF/5 ml H2O/5 ml methanol, was treated with 380 mg of lithium hydroxide hydrate. The mixture was stirred at room temperature 4 hours. The mixture was diluted with 50 ml water and acidified to pH 2 with 1N hydrochloric. The resulting suspension was taken in 100 ml ether and the phases were separated. The aqueous phase was extracted with three portions of 50 ml ether. The combined extracts were dried over MgSO4. The solvent was removed in vacuo and the crude product was purified recrystalization from acetonitrile/water, yielding 796 mg of product as shining platelets. M.p. 74-76° C., [α]D=−22.2 (c=0.500, in CHCl3).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06603012B2 |
| Source dataset | uspto-grants-2003_08 |
| ORD ID | ord-e4ae2b9b0f904544a26b6bcb64bec9d1 |
| Source note | uspto-grants-2003_08 |