HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Methylmorpholine → 1,4-Bis(tert-butoxycarbonyl)-2-formylmethylpiperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Methylmorpholine | HCID 7972 | — |
| Reactant | di-tert-Butyl 2-(2-hydroxyethyl)piperazine-1,4-dicarboxylate | HCID 22710988 | — |
| Catalyst | HCID 178419074 | HCID 178419074 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1,4-Bis(tert-butoxycarbonyl)-2-formylmethylpiperazine | HCID 22710018 | — |
Reaction Steps
In methylene chloride (150 ml) was dissolved 1,4-bis(tert-butoxycarbonyl)-2-(2-hydroxyethyl)piperazine. Under ice cooling, N-methylmorpholine (2.14 g) and tetra-n-propylammonium perruthenate (0.97 g) were added to the reaction mixture, followed by stirring at room temperature for 17 hours. The reaction mixture was then distilled off under reduced pressure. The residue was subjected to chromatography on a silica gel column (hexane:ethyl acetate=9:1 to 2:1), whereby the title compound (3.11 g) was obtained as colorless powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06747023B1 |
| Source dataset | uspto-grants-2004_06 |
| ORD ID | ord-e4e084b2d70246b787df9f9be46e0e48 |
| Source note | uspto-grants-2004_06 |