HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 59558826, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | HCID 67051218 | HCID 67051218 | — |
| Catalyst | Trichloroiron;hexahydrate | HCID 16211236 | — |
| Solvent | Sodium Bicarbonate | HCID 516892 | — |
| Product | HCID 59558826 | HCID 59558826 | — |
Reaction Steps
To a suspension of N-[2-[[(2,3-difluorophenyl)methyl]thio]-6-[1-[(4S)-2,2-dimethyl-1,3-dioxolan-4-yl]-1-methylethoxy]-4-pyrimidinyl]-1-azetidinesulfonamide (the product from step iii) (0.37 g) at DCM (10 mL) was added iron (III) chloride hexahydrate (0.66 g) and the mixture was stirred at ambient temperature for 1 h. The reaction mixture was diluted with sat. sodium hydrogencarbonate solution and extracted with DCM (×3). The combined organic layers were dried (MgSO4), filtered and evaporated. The residue was purified by column chromatography on silica gel using a MeOH/DCM (99:1 to 98:2 gradient) as eluent to give the title compound as a white solid. Yield: 0.16 g
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08722883B2 |
| Source dataset | uspto-grants-2014_05 |
| ORD ID | ord-163816c91c0e42ad9f6fc4031b34ad48 |
| Source note | uspto-grants-2014_05 |