HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 70154633, compound → HCID 53914541, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 70154633 | HCID 70154633 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 53914541 | HCID 53914541 | — |
Reaction Steps
A solution of 3-peroxybenzoic acid (25 g, 102.59 mmol, 2.5 eq.) in anhydrous dichloromethane (250 mL) was added dropwise over a period of one hour to a stirred solution of 8-chloro-4-aza-10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-one 1 (10 g, 41.04 mmol, 1.0 eq.) in anhydrous dichloromethane (100 mL) at 0° C. under a nitrogen atmosphere. The solution was slowly (3 h) warmed to room temperature and stirred for another 12 h. The solution was extracted with 1 M aqueous sodium hydroxide solution (5×100 mL), washed with brine (2×100 mL), dried over Na2SO4, filtered, and concentrated under house vacuum at 30° C. to give 2 as a canary-yellow solid. The title compound 2 was used directly without further attempts at purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06362188B1 |
| Source dataset | uspto-grants-2002_03 |
| ORD ID | ord-45b54a3317f5452da0018265d70bd8df |
| Source note | uspto-grants-2002_03 |