HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromine → HCID 57466726, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | Trifluoroacetate | HCID 84468 | — |
| Reactant | Potassium Bromide | HCID 253877 | — |
| Reactant | HCID 57423980 | HCID 57423980 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 57466726 | HCID 57466726 | — |
Reaction Steps
1.0 g (3.6 mmol) 5,6-dimethyl-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine (as the trifluoroacetate salt) are dissolved in 60 ml of water and at the temperature of an ice bath combined with a solution of 1.0 g (8.5 mmol) potassium bromide and 182 μl (3.6 mmol) bromine in 20 ml of water. The mixture is stirred for 2.5 hours in the ice bath and then extracted twice with 100 ml ethyl acetate. The combined organic phases are washed with sat. sodium chloride solution, then dried on sodium sulphate and evaporated down i. vac. The crude product thus obtained is purified by chromatography on silica gel (eluant DCM/methanol 50:1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08309542B2 |
| Source dataset | uspto-grants-2012_11 |
| ORD ID | ord-022e953da41749cfa28ff4b5d96536dc |
| Source note | uspto-grants-2012_11 |