HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 70040059, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | m-Chloroperbenzoic acid | HCID 70297 | — |
| Reactant | HCID 53873707 | HCID 53873707 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 70040059 | HCID 70040059 | — |
Reaction Steps
4.0 g (10.38 mmol) of t-butyl (S)-11,12,13,13a-tetrahydro-8-methylthio-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate are dissolved in 25 ml of methylene chloride, treated portionwise at room temperature with 2.0 g (about 10.4 mmol) of about 90% percent m-chloroperbenzoic acid and left to stand at room temperature overnight. Then, the solution is poured into 2 N sodium hydroxide, the methylene chloride phase is separated, dried over magnesium sulphate and evaporated. After recrystallization from ethyl acetate/hexane, there is obtained t-butyl (S)-11,12,13,13a-tetrahydro-8-methylsulphinyl-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate of melting point 224°-225° as a diastereoisomeric mixture.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04353827 |
| Source dataset | uspto-grants-1982_10 |
| ORD ID | ord-5cbd725bb6fb40458a2f4f428ca156a9 |
| Source note | uspto-grants-1982_10 |