HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl chloroformate → HCID 86729404, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl chloroformate | HCID 6586 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 86729405 | HCID 86729405 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86729404 | HCID 86729404 | — |
Reaction Steps
4-[4-Carbamoyl-3-({4-[(trifluoromethyl)sulfonyl]phenyl}amino)-1H-pyrazol-1-yl]-4-(cyanomethyl)piperidinium trifluoroacetate (Intermediate #38-7) (30 mg, 0.053 mmol) was dissolved in DCM (1.0 mL). DIPEA (0.055 mL, 0.32 mmol) was added, followed by methyl chloroformate (0.024 mL, 0.32 mmol). The resulting mixture was allowed to stir at ambient temperature for 30 minutes. The solvent was removed in vacuo and the crude residue was purified by reverse-phase preparative HPLC (MeCN/water, with 0.1% v/v TFA modifier). Desired fractions were identified, combined, and concentrated in vacuo to afford the title compound, Example #27-1, as a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09328099B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-1dc7e32be7f24a6e9dd5128abc7acdee |
| Source note | uspto-grants-2016_05 |