HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromine → 2-Bromo-4-(1-methylpiperidin-4-ylidene)-9,10-dihydro-4H-3-thiabenzo[f]azulene hydrobromide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 68491314 | HCID 68491314 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | 2-Bromo-4-(1-methylpiperidin-4-ylidene)-9,10-dihydro-4H-3-thiabenzo[f]azulene hydrobromide | HCID 68488490 | 163.7% |
Reaction Steps
Bromine (0.52 mL, 10.2 mmol) was added dropwise to a chloroform (30 mL) solution of 4-(1-methylpiperidin-4-ylidene)-9,10-dihydro-4H-3-thiabenzo[f]azulene (3.0 g, 10.2 mmol) at 0° C. The mixture was stirred at room temperature for 2 days, and a saturated aqueous sodium bicarbonate solution was then added thereto to allow separation of an organic layer. The organic layer was washed with a saturated sodium chloride solution, and then dried over anhydrous sodium sulfate. The solvents were distilled off under a reduced pressure, and the residue was then purified by column chromatography (chloroform-methanol=9:1), to give 3.8 g (100%) of the captioned compound in the form of white crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08377967B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-b28318d9c0e940dab87ae7356a888387 |
| Source note | uspto-grants-2013_02 |