HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 131724159, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2-chloro-N,N-dimethylacetamide | HCID 75886 | — |
| Reactant | HCID 131724158 | HCID 131724158 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 131724159 | HCID 131724159 | 85.5% |
Reaction Steps
Rac-cis-(3,5-Bis-trifluoromethyl-phenyl)-(3-phenyl-4-piperazin-1-yl-piperidin-1-yl)-methanone (200 mg, 0.41 mmol) was dissolved in N,N-dimethylforamide (5 mL). Potassium carbonate (171 mg, 1.24 mmol) and 2-chloro-N,N-dimethylacetamide (0.042 mL, 0.41 mmol) were added and the reaction mixture was stirred at room temperature overnight. Water (50 mL) was added and the mixture was extracted twice with 100 mL ethyl acetate. Organic phases were pooled, dried with magnesium sulfate and evaporated. Chromatography on silica gel with methylen chloride/methanol/triethyl amine 90:10:1 gave the desired product (200 mg, 85%) as an off-white solid, MS: m/e=571.1 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06642226B2 |
| Source dataset | uspto-grants-2003_11 |
| ORD ID | ord-97188239031c44838578472b34ba2381 |
| Source note | uspto-grants-2003_11 |