HuagongsheHuagongshe Chemistry Print Report · For research reference only
m-Chloroperbenzoic acid → 9-Chloro-7-(2-chlorophenyl)-5H-pyrimido[5,4-d][2]benzazepine-6-oxide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | m-Chloroperbenzoic acid | HCID 70297 | — |
| Reactant | 9-Chloro-7-(2-chlorophenyl)-5H-pyrimido(5,4-d)(2)benzazepine | HCID 131736 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 9-Chloro-7-(2-chlorophenyl)-5H-pyrimido[5,4-d][2]benzazepine-6-oxide | HCID 13202324 | — |
Reaction Steps
A solution of 6.8 g (20 mmole) of 9-chloro-7-(2-chlorophenyl)-5H-pyrimido[5,4-d][2]benzazepine, 6 g (30 mmole) of 85% m-chloroperbenzoic acid in 200 ml of methylene chloride was stirred at room temperature for 4 hrs. The mixture was washed with an excess of ice cold dilute sodium hydroxide, dried over ahydrous sodium sulfate and filtered over hyflo. The filtrate was concentrated at reduced pressure to dryness. The residue was crystallized from a mixture of methylene chloride and ether to give a crude product, mp 228°-229° C. Recrystallization from a mixture of methylene chloride and ether gave the product, mp 216°-217° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04547581 |
| Source dataset | uspto-grants-1985_10 |
| ORD ID | ord-dc83f44845914439b70a6833d6688360 |
| Source note | uspto-grants-1985_10 |