HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 57964191, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 68811174 | HCID 68811174 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 57964191 | HCID 57964191 | 89% |
Reaction Steps
To a cooled solution of 2.5 g (6.25 mmol) of 1-[2-(1,4-dioxaspiro[4.5]dec-8-yl)ethyl]-4-(3-ethoxycarbonylphenyl)piperazine (prepared by path II), is added, under argon, 0.36 g (9.36 mmol) of lithium aluminum hydride. The suspension is stirred overnight at room temperature. Hydrolysis is performed at 0° C. by slow addition of 0.35 mL of water, 0.35 mL of 15% aqueous sodium hydroxide solution and 1.0 mL of water. The slurry is stirred for 15 minutes at room temperature then magnesium sulfate is added. The mixture is filtered and the salts are washed with ethyl acetate. The filtrate is concentrated under reduced pressure to give 2.0 g (89%) of 1-[2-(1,4-dioxaspiro[4.5]dec-8-yl)ethyl]-4-(3-hydroxymethylphenyl)piperazine as a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08802678B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-5090ef274b664bfaa19fe32d42c4daaa |
| Source note | uspto-grants-2014_08 |