HuagongsheHuagongshe Chemistry Print Report · For research reference only
Aluminium lithium hydride → HCID 9863503, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 67636741 | HCID 67636741 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 9863503 | HCID 9863503 | 80.6% |
Reaction Steps
To a mixture of 20.9 g of lithium aluminum hydride and 1000 ml of tetrahydrofuran under ice-cooling and stirring, a solution of 100 g of the compound obtained in Step 1 in 300 ml of tetrahydrofuran was added gradually dropwise at 0°-5° C. and the reaction was carried out at the same temperature for 3 hours. After the excess lithium aluminum hydride was decomposed, the reaction mixture was filtered and the filtrate was concentrated. The residue was dissolved in ethyl acetate and the solution was washed with water, dried, and concentrated to give a white solid. This solid was recrystallized from ethyl acetate, collected by filtration, and dried to provide 74.7 g of the title compound as white crystals. m.p. 171°-173° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05885993 |
| Source dataset | uspto-grants-1999_03 |
| ORD ID | ord-0b8074d2ec6f4375be48b24ba6e61c0e |
| Source note | uspto-grants-1999_03 |