HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine → HCID 57469087, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 60209344 | HCID 60209344 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 57469087 | HCID 57469087 | 92% |
Reaction Steps
To a cooled (ice-water bath) and stirred mixture of methylamine solution (2M in THF) (1.5 ml, 3.0 mmol), triethylamine (0.29 ml, 2.1 mmol) and THF (4 ml) was added drop wise a solution of 3-{4-[4-trifluoromethyl-6-(4-trifluoromethyl-phenyl)-pyrimidin-2-yl]-pyridin-2-yl}-benzenesulfonyl chloride hydrochloride (example I.1) (0.58 g, 1.0 mmol) in THF (6 ml). The mixture was allowed to stir at room temperature for 16 h. Purification of the reaction mixture by flash chromatography on silica gel (ethyl acetate/heptane) and crystallization (dichloromethane/MeOH/hexane) yielded the title compound as a white solid (0.46 g, 92%). MS (ISP) 538.8 [(M+H)+]; mp 174° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08183262B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-130c1a62f9e04933bbaf489cb7e0eb1a |
| Source note | uspto-grants-2012_05 |