HuagongsheHuagongshe Chemistry Print Report · For research reference only
Aluminium lithium hydride → HCID 21928328, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | tert-Butyl (4,4,4-trifluoro-3-hydroxybutyl)carbamate | HCID 21702950 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 21928328 | HCID 21928328 | 61.4% |
Reaction Steps
A solution of (4,4,4-trifluoro-3-hydroxybutyl)carbamic acid tert-butyl ester (0.55 g, 2.26 mmol) in THF (21 mL) was treated with lithium aluminium hydride (0.321 g, 8.46 mmol) at ambient temperature, followed by refluxing for 3 h. The mixture was cooled to ambient temperature and carefully quenched with excess sodium sulphalte decahydrate. Additional THF and diethyl ether were added to aid stirring. The mixture was filtered through a bed of Celite™ and the filtrate was evaporated to a white solid. The solid was purified by silica gel chromatography, eluting with 10% 2M ammonia in methanol/90% dichloromethane and 20% 2M ammonia in methanol/80% dichloromethane (v/v), to give the product as a white solid (0.218 g, 61%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07119109B2 |
| Source dataset | uspto-grants-2006_10 |
| ORD ID | ord-d033a6d9b2434477892bfc458a9fa467 |
| Source note | uspto-grants-2006_10 |