HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloroform → HCID 23084074, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 23138382 | HCID 23138382 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 23084074 | HCID 23084074 | 44% |
Reaction Steps
tert-Butyl 4-((2-hydroxyethyl)((2-methyl-1H-imidazol-5-yl)carbonyl)amino)-1-piperidinecarboxylate (0.94 g) obtained in Example 91b) and triethylamine (0.72 ml) were dissolved in THF (30 ml). Methanesulfonic acid chloride (0.24 ml) was added dropwise under ice-cooling, and then mixed at room temperature for 3 hours. To the reaction solution were added chloroform and water, and the organic layer was collected by separation and dried over anhydrous magnesium sulfate. Then, the solvent was distilled off under reduced pressure, and the residue was purified with basic silica gel column (ethyl acetate:ethanol=5:1) to obtain the title compound as a colorless solid (0.39 g, 44%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07820673B2 |
| Source dataset | uspto-grants-2010_10 |
| ORD ID | ord-01cc56bf466549d8a5c433c9f91854b7 |
| Source note | uspto-grants-2010_10 |