HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → HCID 18461153, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | Piperidine, 1-(2-chloroethyl)-, hydrochloride | HCID 74826 | — |
| Reactant | HCID 18461160 | HCID 18461160 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 18461153 | HCID 18461153 | — |
Reaction Steps
900 mg (2.20 mmol) of [2-(4-methoxyphenyl)-6-methoxybenzo[b]thien-3-yl][3-fluoro-4-hydroxyphenyl]methanone was dissolved in 12 mL of DMF and 810 mg (4.4 mmol) of 1-(2-chloroethyl)piperidine hydrochloride was added. To the reaction mixture was added 3.3 g (10 mmol) of Cs2CO3 and heated to reflux for one hour. The reaction mixture was filtered to remove the solids. The solvents were removed by evaporation and the residue was chromatographed on a silica gel column eluted with a linear gradient of beginning with CHCl3 and ending with MeOH-CHCl3 (1:19). The desired fractions were determined by tlc, combined, and evaporated to a solid. This yielded 960 mg of the title compound as a tan amorphous solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06432982B1 |
| Source dataset | uspto-grants-2002_08 |
| ORD ID | ord-a7da850993e54d3aaff6e1ec926a15a0 |
| Source note | uspto-grants-2002_08 |