HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 1-Benzhydryl-4-(3-methyloxetan-3-yl)piperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Magnesium | HCID 5462224 | — |
| Reactant | 1-Benzhydryl-4-(3-((phenylsulfonyl)methyl)oxetan-3-yl)piperazine | HCID 86708554 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 1-Benzhydryl-4-(3-methyloxetan-3-yl)piperazine | HCID 86708555 | 62.3% |
Reaction Steps
To a suspension of 1-benzhydryl-4-(3-((phenylsulfonyl)methyl)oxetan-3-yl)piperazine (2.49 g, 5.38 mmol) in MeOH (50 mL), THF (10 mL) was added MAGNESIUM (0.654 g, 26.9 mmol) which was pretreated with 1.0 N HCl and rinsed with MeOH, stirred at rt overnight. The Et2O was added and followed by Na2SO4.10H2O, stirred at room temperature for 1 hr, filtered, and filtrate was concentrated. The crude was purified by 40 g ISCO silica column, eluted with EA: HX-0-100%, the desired fractions were concentrated to yield 1-benzhydryl-4-(3-methyloxetan-3-yl)piperazine (1.08 g) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09273057B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-d683b01101584b859730bec77e5c5d31 |
| Source note | uspto-grants-2016_03 |