HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → 3-(4-Fluoro-benzenesulfonyl)-1-trityloxy-azepan-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | N-(4-Bromo-butyl)-2-(4-fluoro-benzenesulfonyl)-N-trityloxy-acetamide | HCID 86619941 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 3-(4-Fluoro-benzenesulfonyl)-1-trityloxy-azepan-2-one | HCID 68513693 | — |
Reaction Steps
N-(4-Bromo-butyl)-2-(4-fluoro-benzenesulfonyl)-N-trityloxy-acetamide prepared from step E (170.2 mg, 0.279 mmol) and Cs2CO3 (187.3 mg, 0.575 mmol) in anhydrous DMF (6 mL) was stirred at room temperature for overnight.). The reaction mixture was diluted with EtOAc and washed sequentially with water and saturated NaCl solution. The organic phase was then dried over anhydrous Na2SO4 and concentrated under reduced pressure to gave a crude material, which was then purified by a column chromatography (0˜30% EtOAc in hexane). MS: 552.2 (M+Na)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07803793B2 |
| Source dataset | uspto-grants-2010_09 |
| ORD ID | ord-538f2771775c4235847da2d0a58d9187 |
| Source note | uspto-grants-2010_09 |