HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 70270704, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 57144221 | HCID 57144221 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 70270704 | HCID 70270704 | 90.8% |
Reaction Steps
In a 50 ml flask were charged 1.2 g of lithium aluminum hydride and 50 ml of THF, and a solution of 7.85 g of the compound obtained in Step 2 in 20 ml of THF was added thereto dropwise under ice-cooling, followed by stirring at room temperature for 1 hour. Then, 1.2 ml of water and 20 ml of THF were added thereto dropwise over 15 minutes. To the reaction mixture was further added dropwise 3.6 ml of a 4% sodium hydroxide aqueous solution under cooling with ice over 40 minutes, followed by filtration through zeolite. The filtrate was distilled under reduced pressure to remove the solvent, and the resulting crude product was purified by silica gel column chromatography to obtain 5.9 g (20.9%) of the titled compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06093345 |
| Source dataset | uspto-grants-2000_07 |
| ORD ID | ord-3cac3625d08c401982e9aa1ca5cd989e |
| Source note | uspto-grants-2000_07 |