HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 25196150, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Trifluoroacetic acid methylene chloride | HCID 21863450 | — |
| Reactant | HCID 86657486 | HCID 86657486 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 25196150 | HCID 25196150 | — |
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 (55.5 mg, 0.128 mmol) in dichloromethane (5 mL) at room temperature, triethylamine (0.045 mL, 0.320 mmol) and methanesulfonyl chloride (0.011 mL, 0.147 mmol) were added. The mixture was stirred for 1 h at room temperature. The residue was purified by prep TLC on silica gel, eluting with EtOAc/MeOH/NH4OH (90/9/1) to give first eluting isomer as isomer A and second eluting isomer as isomer B. Isomer A was treated with TFA/CH2Cl2=1:1 for 1 h to give the title compound. (LC-MS: 411.92 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08653059B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-d54b8477714e4fc6b23b5412cb3022d9 |
| Source note | uspto-grants-2014_02 |