HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 68931295, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 68734777 | HCID 68734777 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 68931295 | HCID 68931295 | 97.4% |
Reaction Steps
A solution of LiAlH4 (1.5 mL, 1.5 mmol, 1 M/THF) was added to a 0° C. solution of 5-4 (453 mg, 1.34 mmol) in THF (5 mL). After 3 h, H2O (5 mL) was added dropwise followed by dichloromethane and 15% NaOH (10 mL). The reaction was allowed to warm to room temperature and was stirred further for 30 min. The resulting mixture was extracted with dichloromethane (3×) and the combined dichloromethane solution was dried (Na2SO4), filtered and evaporated. Purification of the residue by flash chromatography on silica gel (Isco Combiflash unit) gave the title compound (447 mg, 97%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09006464B2 |
| Source dataset | uspto-grants-2015_04 |
| ORD ID | ord-90ad297966f044e3b1d87590c173062c |
| Source note | uspto-grants-2015_04 |