HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 22110967, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 22110983 | HCID 22110983 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 22110967 | HCID 22110967 | 64.7% |
Reaction Steps
To a solution of N-[2,3-dihydro-2,4,6,7-tetramethyl-2-[(4-phenyl-1-piperidinyl)methyl]benzofuran-5-yl]acetamide (0.56 g) in tetrahydrofuran (8 mL) was added 0.11 g of lithium aluminum hydride in small portions under ice-cooling. The mixture was then refluxed for 30 hours. After this reaction mixture was cooled with ice, 0.42 g Hyflo Super-Cel (tradename) and ethyl acetate were added, further followed by addition of water (0.2 mL). The mixture was stirred vigorously and, then, filtered and the filtrate was concentrated under reduced pressure. The residue was subjected to silica gel column chromatography (hexane:ethyl acetate=5:1) to provide 0.35 g of the title compound. Yield 63%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06172085B2 |
| Source dataset | uspto-grants-2001_01 |
| ORD ID | ord-1735eeb7addd4e86b4a53575fc924b10 |
| Source note | uspto-grants-2001_01 |