HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonyl chloride → HCID 68693526, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 24760585 | HCID 24760585 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | Sodium Bicarbonate | HCID 516892 | — |
| Product | HCID 68693526 | HCID 68693526 | 29.4% |
Reaction Steps
To a stirred and cooled solution of 3-[6-methyl-4-(4-trifluoromethyl-phenyl)-[2,4′]bipyridinyl-2′-yl]-phenylamine (example 307) (0.200 g, 0.493 mmol) in EtOAc (2 mL) and sat. NaHCO3-sol. (1 mL) was added methanesulfonyl chloride (1.0 mL, 13.6 mmol) and the mixture was stirred at 23° C. for 2 h. Diluted with EtOAc, washed with sat. NaHCO3-sol. and water, dried the organic layer over Na2SO4. Removal of the solvent in vacuum left a crude product which was purified by silica gel column chromatography with EtOAc, followed by trituration with diethyl ether to give the title compound as a white solid (0.070 g, 29%). MS (ISP) 484.4 [(M+H)+]; mp 196° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08183262B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-7e60963349324f4aa9a789faa3e0a41b |
| Source note | uspto-grants-2012_05 |