HuagongsheHuagongshe Chemistry Print Report · For research reference only
Aluminium lithium hydride → HCID 59828837, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 59828831 | HCID 59828831 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59828837 | HCID 59828837 | 82% |
Reaction Steps
Add a solution of 1M lithium aluminum hydride in THF (4.6 mL, 4.6 mmol) over 5 min to a solution of 4-(2-cyclopropylmethylamino-5-methyl-thiazol-4-yl)-benzonitrile (410 mg, 1.52 mmol) in anhydrous THF (10 mL). Heat to reflux for 30 min, cool to room temperature and quench by dropwise addition of water (5 mL), ether (50 mL), 3N NaOH (5 mL) and additional water (15 mL). Stir vigorously for 30 min and filter over a bed of Celite®. Wash the filtrate with water (2×100 mL) and brine (100 mL). Dry the organic phase over MgSO4, filter and concentrate in vacuo to obtain the title compound as a yellow oil (340 mg, 82%) that was used without further purification. MS (ES+) m/z: 274 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08680091B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-7b98979526734fcfbd5f6db7788cf412 |
| Source note | uspto-grants-2014_03 |