HuagongsheHuagongshe Chemistry Print Report · For research reference only
Aluminium lithium hydride → HCID 58303926, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 58303937 | HCID 58303937 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 58303926 | HCID 58303926 | 23% |
Reaction Steps
To a solution of 29-3 (100 mg, 0.24 mmol) in THF (10 mL) was added lithium aluminum hydride (19 mg, 0.48 mmol). The mixture was stirred at room temperature overnight. Na2SO4.10H2O was added and the reaction mixture was filtered and the filtrate was evaporated to give the crude product which was purified by preparative HPLC (basic condition, water/CH3CN, 43-53% CH3CN in 7.5 min, RT=7.3 min) to afford 29-4 (22 mg, 23%) as a yellow solid. 1H-NMR (400 MHz, CDCl3): δ (ppm) 7.52-7.50 (br.s, 2H), 7.20-7.16 (m, 2H), 6.76 (s, 1H), 6.66 (d, J=12.8 Hz, 1H), 3.96 (q, J=7.2 Hz, 2H), 3.81 (s, 3H), 3.14 (t, J=7.2 Hz, 2H), 3.06-2.98 (m, 4H), 2.69 (t, J=7.6 Hz, 2H), 2.38 (s, 6H) 1.30 (t, J=7.2 Hz, 3H). LRMS: calc 408.5 and found: 409.2 [M+1].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08912220B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-5987c243c50e4e7b8acd6ff7583c702e |
| Source note | uspto-grants-2014_12 |