HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Hydroxide → 2-Benzo[1,3]dioxol-5-ylmethyl-1-tert-butoxycarbonylpiperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | 2-Benzo[1,3]dioxol-5-ylmethyl-1-tert-butoxycarbonyl-3-oxopiperazine | HCID 23155909 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2-Benzo[1,3]dioxol-5-ylmethyl-1-tert-butoxycarbonylpiperazine | HCID 23155618 | 66.3% |
Reaction Steps
Dissolving 2.00 g of 2-benzo[1,3]dioxol-5-ylmethyl-1-tert-butoxycarbonyl-3-oxopiperazine as synthesized in the above step in 50 ml of tetrahydrofuran, 1.00 g of lithium aluminium hydride was added to the solution which then was heated under reflux for 16 hours. To the solution 10% aqueous potassium hydroxide solution was added, the insoluble matter was filtered off, extracted with ethyl acetate, the extract was dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure. The residue was purified on silica gel column chromatography (methanol:chloroform=1:19) to provide 1.27 g (66%) of 2-benzo[1,3]dioxol-5-ylmethyl-1-tert-butoxycarbonylpiperazine.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07799775B2 |
| Source dataset | uspto-grants-2010_09 |
| ORD ID | ord-30d5f4a6f16e45f4873d184662d36bc2 |
| Source note | uspto-grants-2010_09 |