HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 52951616, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 52951277 | HCID 52951277 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 52951616 | HCID 52951616 | 85% |
Reaction Steps
To a solution of ester 17 (1.27 g, 4 mmol) in 40 mL of THF was added LiAlH4 (0.24 mg, 6.4 mmol). The reaction mixture was stirred for 6 hours at room temperature. EtOAC (5 mL) and water (10 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=7:3) to give the titled compound (0.97 g, 85%) as a white solid mp 119.5-123.4° C. 1H NMR (300 MHz, DMSO-d6): δ 7.91 (d, J=9 Hz, 2H), 7.46 (d, J=9 Hz, 2H), 7.43-7.37 (m, 3H), 7.31-7.25 (m, 2H), 6.56 (s, 1H), 4.52 (t, J=5 Hz, 1H), 3.54-3.46 (m, 2H), 3.24 (s, 3H), 2.79-2.60 (m, 2H), 1.88-1.77 (m, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09096532B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-f0a53c69d5b943c2bef31017f868041c |
| Source note | uspto-grants-2015_08 |