HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine → HCID 18542698, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Isobutyl chloroformate | HCID 62365 | — |
| Reactant | HCID 22181141 | HCID 22181141 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 18542698 | HCID 18542698 | — |
Reaction Steps
To a solution of 4-(1-t-butoxycarbonylpiperidin-4-yloxy)-3-carboxynitrobenzene (3.3 g) in dichloromethane (50 ml) were added isobutyl chloroformate (1.4 ml) and triethylamine (1.4 ml) in an ice bath and the mixture was stirred at the same temperature for 0.5 hours. To the reaction mixture was added 40% aqueous methylamine (1.1 ml) and the resulting mixture was stirred at room temperature for 3 hours. The reaction mixture was concentrated in vacuo. The residue was purified by chromatography on a silica gel column using dichloromethane/methanol=19/1 as an eluant to give the desired compound (3.5 g, yield quantitative) as a yellow amorphous solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06555556B1 |
| Source dataset | uspto-grants-2003_04 |
| ORD ID | ord-f93964506ef746989c479529f50ebc93 |
| Source note | uspto-grants-2003_04 |