HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → HCID 22993353, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 22993363 | HCID 22993363 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 22993353 | HCID 22993353 | — |
Reaction Steps
Under an inert atmosphere, the compound obtained in Step B (3.26 g; 12.77 mmol) is dissolved in 70 ml of anhydrous tetrahydrofuran (6 ml/1 mmol), and then lithium aluminium hydride (5 eq.; 63.85 mmol; 2.42 g) is added in portions at 0° C. The mixture is stirred at ambient temperature for 16 hours, and then the solution is hydrolysed at 0° C. with 2.4 ml of water, 2.4 ml of a 15% sodium hydroxide solution and 7.2 ml of water. The solution is stirred for 30 minutes, and the salts that have formed are filtered off using a Büchner funnel and the solvent is removed under reduced pressure. The crude reaction product is purified by flash chromatography on silica gel (eluant: PE/AcOEt (8/2)). The title product is obtained in the form of a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06620809B2 |
| Source dataset | uspto-grants-2003_09 |
| ORD ID | ord-7243c222eee64ab3a5503f94031f05cc |
| Source note | uspto-grants-2003_09 |