HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 6-Bromoisoquinoline N-oxide hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | m-Chloroperbenzoic acid | HCID 70297 | — |
| Reactant | 6-Bromoisoquinoline | HCID 313681 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 6-Bromoisoquinoline N-oxide hydrochloride | HCID 22665630 | 90.8% |
Reaction Steps
To a stirred solution of 13.2 g of 6-bromoisoquinoline (Tyson, F. L., J. Am. Chem. Soc. 61, 183 (1939)) in 250 mL of dichloromethane at room temperature was added in portions 16.2 g of m-chloroperbenzoic acid (purity 70%). After stirring the mixture for one hour 200 mL of methanol was added and the bulk was reduced to 150 mL. A hydrogen chloride solution in methanol (100 mL, 0.75 M) was added and after slightly heating a clear solution was obtained. Diethylether (250 mL) was added to this solution and cooled in an ice bath. The hydrochloride salt precipitated and was isolated by filtration to give 15 g of 1a. M.p. 194-196° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06797710B2 |
| Source dataset | uspto-grants-2004_09 |
| ORD ID | ord-e3cf6d9ecbed4c8bb92096f4370ba072 |
| Source note | uspto-grants-2004_09 |