HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Acetate → acetic acid-(4S)-{[2-(4-ethyl-4-hydroxy-3,13-dioxo-3,4,12,13-tetrahydro-1H-2-oxa-6,12a-diaza-dibenzo[b,h]fluoren-11-yl)-ethyl]-dimethylsilanyl}-methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Acetate | HCID 517044 | — |
| Reactant | 11-(4S)-[2-(chloromethyldimethylsilanyl)-ethyl]-4-ethyl-4-hydroxy-1,12-dihydro-4H-2-oxa-6,12a-diaza-dibenzo[b,h]fluorene-3,13-dione | HCID 25227497 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | acetic acid-(4S)-{[2-(4-ethyl-4-hydroxy-3,13-dioxo-3,4,12,13-tetrahydro-1H-2-oxa-6,12a-diaza-dibenzo[b,h]fluoren-11-yl)-ethyl]-dimethylsilanyl}-methyl ester | HCID 25260766 | 72% |
Reaction Steps
A solution of Compound 3 (200 mg) and potassium acetate (200 mg) in dry N,N-dimethylformamide (4 mL) was heated at 80° C. for 16 hours. The reaction mixture was cooled to room temperature and the N,N-dimethylformamide was removed under vacuum with mild heating. The obtained crude material was directly purified on a silica gel column using 1-2% ethanol in dichloromethane to obtain the required product in 72% yield (150 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07687496B2 |
| Source dataset | uspto-grants-2010_03 |
| ORD ID | ord-c1e0ba87fc1e474990dbd981354feaa6 |
| Source note | uspto-grants-2010_03 |