HuagongsheHuagongshe Chemistry Print Report · For research reference only
Piperazine → Piperazine, 1,4-bis(1,3-benzodioxol-5-ylmethyl)-
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Piperazine | HCID 4837 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 1,3-Benzodioxole, 5-(chloromethyl)- | HCID 88713 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | Piperazine, 1,4-bis(1,3-benzodioxol-5-ylmethyl)- | HCID 96702 | — |
Reaction Steps
To a solution of piperazine (207 mg) in dry DMF (5 ml) under nitrogen was added sodium hydride (80% w/w in oil, 250 mg), followed by 3,4-methylenedioxybenzylchloride (0.90 g) and the mixture stirred at room temperature overnight. Aqueous NaOH (50 ml, 1M) was added slowly, then saturated NaCl solution (50 ml) and the product extracted with dichloromethane (2×100 ml). The organic layer was washed with water (2×100 ml), dried and evaporated in vacuo to give a white solid. Column chromatography eluting with increasing proportions of ether in dichloromethane gave pure DC-0009B (0.68 g, 80%) as a white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08895554B2 |
| Source dataset | uspto-grants-2014_11 |
| ORD ID | ord-b6a3b3bbcf734e9fb879bf5cafc2f30a |
| Source note | uspto-grants-2014_11 |