HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 25196492, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Trifluoromethanesulfonyl chloride | HCID 79000 | — |
| Reactant | Trifluoroacetic acid methylene chloride | HCID 21863450 | — |
| Reactant | HCID 86657486 | HCID 86657486 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 25196492 | HCID 25196492 | — |
Reaction Steps
To a solution of tert-butyl [(2R,3S,5R)-2-(2,5-difluorophenyl)-5-(4,6-dihydropyrrolo[3,4-c]pyrazol-5(1H)-yl)-1-methyl-6-oxopiperidin-3-yl]carbamate (60 mg, 0.138 mmol) in dichloromethane (4 mL) at room temperature, triethylamine (0.048 mL, 0.346 mmol) and trifluoromethanesulfonyl chloride (0.029 mL, 0.277 mmol) were added. The mixture was stirred overnight at room temperature. The residue was purified by preparative TLC on silica gel, eluting with CH2Cl2/MeOH/aqueous NH3 (95/4/1) to give first eluting isomer as isomer A and second eluting isomer as isomer B. Isomer A was treated with 1:1 TFA/CH2Cl2 for 1 h to give the title compound. LC-MS: 465.84 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08653059B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-c83fc083a5a945bc8954168edb4cbb41 |
| Source note | uspto-grants-2014_02 |