HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 68819643, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 17755035 | HCID 17755035 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 68819643 | HCID 68819643 | 798% |
Reaction Steps
To a solution of compound 3c (4 g, 1.04 mmol) in 20 mL of THF was added LiAlH4 (1.26 g, 33.2 mmol). The reaction mixture was stirred for 6 hours at room temperature. EtOAC (30 mL) and water (30 mL) were added successively. The solvent was removed in vacuo and the resulting solid was filtered. The crude product was purified by column chromatography (EtOAc/Hexanes in adequate proportions) to give the compound (2.85 g, 80%) as a white solid. mp 165.9-169.3° C. 1H NMR (300 MHz, DMSO-d6): δ 7.81 (d, J=9 Hz, 2H), 7.48-7.43 (m, 2H), 7.41 (d, J=9 Hz, 2H), 7.21 (d, J=8 Hz, 2H), 7.14 (d, J=8 Hz, 2H), 6.59 (s, 1H), 5.26 (t, J=6 Hz, 1H), 4.51 (d, J=6 Hz, 2H), 2.31 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09096532B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-313846c440874bbaaa4a13a60bda51ea |
| Source note | uspto-grants-2015_08 |