HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sch 37370 → HCID 22914781, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sch 37370 | HCID 60680 | — |
| Reactant | m-Chloroperbenzoic acid | HCID 70297 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22914781 | HCID 22914781 | 29.7% |
Reaction Steps
To a mixture of 711 mg (2.01 mmole) of 8-chloro-11-(1-acetyl-4-piperidylidene)-6,11-dihydro-5 H-benzo[5,6]cyclohepta[1,2-b]pyridine in 30 ml of dry CH2Cl2 at -10° C. and under a nitrogen atmosphere was added 246 mg (1.60 mmole) of m-chloroperoxybenzoic acid. After 95 min. the mixture was taken up in CH2Cl2 and washed once with 10% aqueous sodium bisulfite and once with 10% aqueous sodium hydroxide. It was dried over magnesium sulfate, filtered, and concentrated in vacuo. The product was purified via flash chromatography (MeOH in CH2Cl2) and recrystallized from ethyl acetateexanes to give 175 mg of the title compound as a hemi-ethyl acetate solid. (m.p. 90.5°-93° C.)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05665726 |
| Source dataset | uspto-grants-1997_09 |
| ORD ID | ord-a2ccaac3f00d4e91adcc98290436e93c |
| Source note | uspto-grants-1997_09 |