HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 9912262, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 5311125 | HCID 5311125 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 9912262 | HCID 9912262 | 68.6% |
Reaction Steps
To a solution of 4-(4-chlorophenyl)-1-[3-(11-cyano-6,11-dihydrodibenzo[b,e]thiepin-11-yl)propyl]piperidin-4-ol (430 mg) in THF (10 ml) was added 1M lithium aluminum hydride THF solution (1.5 ml) and the mixture was heated to reflux for 3 hours. The reaction mixture was cooled with ice, water (0.06 ml), then 15% aqueous sodium hydroxide (0.06 ml), then water (0.18 ml) were added carefully. The granular salt was filtered off and the filtrate was distilled off under reduced pressure. The residue was purified by silica gel chromatography eluting with ethyl acetate-hexane (1:1) to give the titled compound (280 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06433165B1 |
| Source dataset | uspto-grants-2002_08 |
| ORD ID | ord-cf2d07be84cb47d59549aa0fdf8c4b4a |
| Source note | uspto-grants-2002_08 |