HuagongsheHuagongshe Chemistry Print Report · For research reference only
N-bromobutanimide → 1-Bromo-4-hydroxy-8-phenoxy-isoquinoline-3-carboxylic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | 4-Hydroxy-8-phenoxy-isoquinoline-3-carboxylic acid methyl ester | HCID 67110848 | — |
| Catalyst | Benzoyl Peroxide | HCID 7187 | — |
| Solvent | Carbon Tetrachloride | HCID 5943 | — |
| Product | 1-Bromo-4-hydroxy-8-phenoxy-isoquinoline-3-carboxylic acid methyl ester | HCID 86617062 | 97.7% |
Reaction Steps
A mixture of 4-hydroxy-8-phenoxy-isoquinoline-3-carboxylic acid methyl ester (103 mg, 0.35 mmol), N-bromosuccinimide (65 mg, 0.37 mmol), benzoyl peroxide (4.2 mg, 0.02 mmol), and carbon tetrachloride (2.5 mL) was refluxed for 4 h before it was cooled to room temperature and filtered. The filtrate was washed with water, saturated aqueous sodium bicarbonate solution, and brine before it was dried over anhydrous sodium sulfate and concentrated in vacuo to give the title compound as a yellow solid (128 mg): MS: (+) m/z 374.0, 376.0 (M+1, 79Br/81Br), MS: (−) m/z 372.1, 374.1 (M−1, 79Br/81Br).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09174976B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-d6fcb279a53145c5a42a39975839d4f5 |
| Source note | uspto-grants-2015_11 |