HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 3-Chloro-4-fluorobenzo[b]thiophene-7-carbonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2,3-Dichloro-4-fluoro-2,3-dihydrobenzo[b]thiophene-7-carbonitrile | HCID 68546843 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-Chloro-4-fluorobenzo[b]thiophene-7-carbonitrile | HCID 68549486 | — |
Reaction Steps
Triethylamine (1.70 mL, 12.2 mmol) was added to a solution of 2,3-dichloro-4-fluoro-2,3-dihydrobenzo[b]thiophene-7-carbonitrile (1.57 g, 5.93 mmol) in dichloromethane (50 mL). The mixture was stirred at room temperature for 7 days, then the solvent was removed and the residue extracted with EtOAc. The organic extracts were then washed with water, brine and dried over Na2SO4. After removal of the solvent, the residue was purified by silica gel column chromatography to give 3-chloro-4-fluorobenzo[b]thiophene-7-carbonitrile as a white solid (1.19 g, 95% for two steps). 1H NMR (400 MHz, CDCl3, δ in ppm) 7.73 (dd, J=4.1, 8.2 Hz, 1H), 7.42 (s, 1H), 7.17 (dd, J=8.2, 10.5 Hz, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08268872B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-23ff02013fda4a2aa73088724b15be4b |
| Source note | uspto-grants-2012_09 |