HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Peroxide → HCID 13280942, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Peroxide | HCID 784 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | HCID 13067111 | HCID 13067111 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ammonium Hydroxide | HCID 14923 | — |
| Product | HCID 13280942 | HCID 13280942 | — |
Reaction Steps
In one portion, 1 ml of 30% hydrogen peroxide was added to 40 ml of a 1% solution of concentrated sulfuric acid in acetic acid. After stirring for 1 hour, 2.0 g (5.8 mmol) of 8-chloro-6-(2-chlorophenyl)-1-methyl-2H,4H-pyrrolo[3,4-d][2]benzazepine were added, and the resulting mixture was stirred at room temperature for 30 minutes. The mixture was diluted with methylene chloride and neutralized with concentrated ammonium hydroxide solution. The methylene chloride solution was dried over anhydrous sodium sulfate and concentrated at reduced pressure to a dark residue. Crystallization from ethyl acetate gave 8-chloro-6-(2-chlorophenyl)-1,4-dihydro-1-methylpyrrolo[3,4-d][2]benzazepin-3(2H)-one as pale yellow prisms, mp 239°-241° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04436662 |
| Source dataset | uspto-grants-1984_03 |
| ORD ID | ord-9f9f74059eff4edeb0c704c4b30f24cd |
| Source note | uspto-grants-1984_03 |