HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → HCID 57420348, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | HCID 1122381 | HCID 1122381 | — |
| Reactant | HCID 178418573 | HCID 178418573 | — |
| Catalyst | Zirconium chloride (ZrCl4), (T-4)- | HCID 9856075 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 57420348 | HCID 57420348 | — |
Reaction Steps
To a solution of 1-(4-benzyl-piperazin-1-yl)-2-methoxy-ethanone (6.14 g) in dry THF (80 mL) at −10° C. was added zirconium chloride (5.76 g). After 30 minutes methyl magnesium bromide (3.0M solution in ether, 49.6 mL) was added in a dropwise manner. The reaction mixture was allowed to warm to room temperature. After stirring for 1 day, the reaction mixture was cooled, diluted with chloroform, washed with brine, dried (MgSO4) and the was solvent removed in vacuo. The resulting residue was purified using flash chromatography to yield 1-benzyl-4-(2-methoxy-1,1-dimethyl-ethyl)-piperazine. Subsequent transfer hydrogenation, using ammonium formate and 10% palladium on carbon in MeOH, furnished the desired compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07750002B2 |
| Source dataset | uspto-grants-2010_07 |
| ORD ID | ord-72db30093a4e48339e1713d4568a3f5b |
| Source note | uspto-grants-2010_07 |