HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → HCID 10304406, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 2-(3,5-bis-trifluoromethyl-phenyl)-N-methyl-N-(6-thiomorpholin-4-yl-4-o-tolyl-pyridin-3-yl)-isobutyramide | HCID 11250186 | — |
| Reactant | Sodium Bisulfite | HCID 23665763 | — |
| Reactant | Potassium hydroxy sulfite | HCID 23707502 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 10304406 | HCID 10304406 | 93% |
Reaction Steps
To a solution of 1.00 g (1.72 mmol) 2-(3,5-bis-trifluoromethyl-phenyl)-N-methyl-N-(6-thiomorpholin-4-yl-4-o-tolyl-pyridin-3-yl)-isobutyramide in 10 ml methanol were added 1.59 g (2.58 mmol) OXONE®. After stirring for 2 days at room temperature, 5 ml 38% sodium hydrogensulfite solution and 20 ml saturated sodium carbonate solution were added consecutively and methanol was removed in vacuo. The residue was diluted with 25 ml water and extracted with three 25-ml portions of dichloromethane. The combined organic layers were dried (sodium sulfate), purified by flash chromatography and crystallized from ethanol to give 980 mg (93%) of the title compound as white crystals. M.p. 200-201° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06849624B2 |
| Source dataset | uspto-grants-2005_02 |
| ORD ID | ord-2318b35b29504f0ba66fc5ea24422cc2 |
| Source note | uspto-grants-2005_02 |