HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonyl chloride → LGX-818
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | CarbaMic acid, N-[(1S)-2-[[4-[3-(3-aMino-5-chloro-2-fluorophenyl)-1-(1-Methylethyl)-1H-pyrazol-4-yl]-2-pyriMidinyl]aMino]-1-Methylethyl]-, Methyl ester | HCID 70313839 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | LGX-818 | HCID 50922675 | — |
Reaction Steps
Methanesulfonyl chloride (0.277 mL, 3.57 mmol) was added to a solution of (S)-methyl 1-(4-(3-(3-amino-5-chloro-2-fluorophenyl)-1-isopropyl-1H-pyrazol-4-yl)pyrimidin-2-ylamino)propan-2-ylcarbamate (550 mg, 1.2 mmol) in DCM (30 mL) and pyridine (10 mL), and the mixture was stirred at rt for 16 h. Aqueous sodium bicarbonate solution was added, and the mixture was extracted with ethyl acetate and washed with brine. The organic phase was dried over sodium sulfate and concentrated. The crude product was purified by silica gel chromatography (60:1 to 40:1 DCM/methanol) to provide the title compound. An alternative synthesis is described in example 6, infra.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09314464B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-8e192829b4274d54a4f189ca54b8c079 |
| Source note | uspto-grants-2016_04 |