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-5H-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 acetate/hexanes 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 | US05089496 |
| Source dataset | uspto-grants-1992_02 |
| ORD ID | ord-5cae7c6ec94e4ad3b6a2f4f0e9ac95de |
| Source note | uspto-grants-1992_02 |