HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 67000197, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 67000042 | HCID 67000042 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 67000197 | HCID 67000197 | 92% |
Reaction Steps
Stir a mixture of (S)—N—((R)-1-(2-((2-(2-(2-(1H-1,2,3-Triazol-1-yl)ethylamino)-5-fluoropyrimidin-4-yl)benzo[b]thiophen-7-yl)methyl)-4-fluorophenyl)-2,2,2-trifluoroethyl)-2-methylpropane-2-sulfinamide (10.5 g, 16.52 mmol) and HCl (16.52 mL, 66.07 mmol, in dioxane) in methanol (100 mL) for 2 h. Concentrate the mixture and dilute with NaOH (1 N). Extract the product with ethyl acetate (150 mL×3). Wash the organic layer with 1:1 water/aqueous saturated sodium chloride and aqueous saturated sodium chloride. Dry over Na2SO4, filter, and concentrate. Dissolve the material with heat in DCM/hexanes and solidify the material in 3 h upon cooling. Filter the solid to give the title compound (8.1 g tan solid, 92%). MS (ES) m/z 546 [M+1]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08063035B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-0268ad85b3864f748c9863fcd6e5dfd7 |
| Source note | uspto-grants-2011_11 |