HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Methylimidazole → HCID 118661240, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Methylimidazole | HCID 1390 | — |
| Reactant | 4-Toluenesulfonyl chloride | HCID 7397 | — |
| Reactant | Edoxaban Impurity 158 | HCID 118671017 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 118661240 | HCID 118661240 | 38% |
Reaction Steps
t-Butyl {[(1R,2R,5S)-5-(dimethylcarbamoyl)-2-hydroxycyclohexyl]sulfamoyl}carbamate (200 mg) was dissolved in dichloromethane (2.0 mL), and p-toluenesulfonyl chloride (136 mg) and N-methylimidazole (87.0 mL) were then added to the obtained solution. The obtained mixture was stirred at room temperature for approximately 20 hours. Thereafter, the reaction mixture was purified by silica gel column chromatography to obtain the title compound (107 mg, yield: 38%) in the form of powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09447118B2 |
| Source dataset | uspto-grants-2016_09 |
| ORD ID | ord-b4e7473e492f48f7becd710944484f7d |
| Source note | uspto-grants-2016_09 |