HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → HCID 69053505, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 2-(2-Bromoethyl)-1,3-dioxolane | HCID 87776 | — |
| Reactant | HCID 69055364 | HCID 69055364 | — |
| Product | HCID 69053505 | HCID 69053505 | 46.8% |
Reaction Steps
A mixture of 2-(2-bromoethyl)-1,3-dioxolane (0.04 mol), intermediate (6) (0.04 mol) and Na2CO3 (10%, 0.08 mol) in MIK (400 ml) was stirred and refluxed for 20 hours and then cooled. The solvent was evaporated. The residue was taken up in DCM and water. The organic layer was separated, dried, filtered and the solvent was evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2C2/(CH3OH/NH3) 96/4). The pure fractions were collected and the solvent was evaporated. Toluene was added and evaporated again, yielding 6 g of (trans)-1-[2-(1,3-dioxolan-2-yl)ethyl]-4-[[(phenylmethyl)amino]methyl]-3-piperidinol (intermediate 7).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06544997B1 |
| Source dataset | uspto-grants-2003_04 |
| ORD ID | ord-8b83838dd4764d34b12d539b3f614074 |
| Source note | uspto-grants-2003_04 |