HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → 4-Bromo-3-methyl-isoquinoline
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 3-Methylisoquinoline | HCID 14306 | — |
| Reactant | Bromine | HCID 24408 | — |
| Solvent | Nitrobenzene | HCID 7416 | — |
| Product | 4-Bromo-3-methyl-isoquinoline | HCID 3777703 | 72.3% |
Reaction Conditions
| Temperature | 180 °C |
|---|
Reaction Steps
To 3-methylisoquinoline (0.500 g, 3.49 mmol) in 1 ml nitrobenzene, bromine (0.196 ml, 3.84 mmol) was added and the contents heated in a sealed tube at 180° C. for 4 hours. The solution was cooled to room temperature, neutralized with solid sodium carbonate (pH=8) and extracted with ethyl acetate (2×20 ml). The organic layer was dried over sodium sulfate, filtered, concentrated and column purified (hexane:EtOAc; 4.5:0.5) to give 0.560 g (72%) of the product as syrup.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06777426B2 |
| Source dataset | uspto-grants-2004_08 |
| ORD ID | ord-dd99a739806f43e796998e1b36f4a0a0 |
| Source note | uspto-grants-2004_08 |