HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 67133585, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1-(3-Bromopropyl)-4-fluorobenzene | HCID 14737133 | — |
| Reactant | HCID 178524460 | HCID 178524460 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | Ethyl acetate hexane | HCID 21226206 | — |
| Product | HCID 67133585 | HCID 67133585 | 47% |
Reaction Steps
4.9 g (35.8 mmol) of K2CO3 were added to a solution of 2.5 g (16.3 mmol) of 2-mercapto-nicotinic acid in DMF (40 ml), and the mixture was stirred for 30 min at RT. 3.5 g (16.3 mmol) of 1-(3-bromopropyl)-4-fluorobenzene were then added and stirring was carried out for a further 72 h at RT. The mixture was then diluted with water and EA and adjusted to pH 5-6 with 5M acetic acid. The organic phase was separated off, washed with water, dried over MgSO4, filtered and concentrated in vacuo. CC (EA/hexane 1:2→5:1) of the residue yielded 2.2 g (7.6 mmol, 47%) of 2-(3-(4-fluoro-phenyl)propylthio)nicotinic acid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08178684B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-778390705356493ba3a6afd7e98f336b |
| Source note | uspto-grants-2012_05 |