HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium aluminum hydride → HCID 58204257, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium aluminum hydride | HCID 28112 | — |
| Reactant | HCID 58204053 | HCID 58204053 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 58204257 | HCID 58204257 | 47.2% |
Reaction Steps
To a solution of 2-(2-Isopropyl-5-methyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulene-8-carbonitrile (0.500 g, 0.00142 mol) in Tetrahydrofuran (14 mL) was added Lithium tetrahydroaluminate (0.00569 mol, 1M in THF, 5.7 mL), dropwise at 0° C. The reaction was stirred for 2 hours and quenched with saturated Na2SO4 until H2 evolution ceased. MgSO4 was added and the whole was diluted with copious amounts of methylene chloride, filtered over celite, and concentrated in vacuo. The crude was purified by flash chromatography (1-15% MeOH in DCM spiked with Et3N) to afford 532 as a yellow solid (238 mg). MS(ESI+) 356.1
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09175009B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-fe1a46437b8748088bb6b2984e58ed9e |
| Source note | uspto-grants-2015_11 |