HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178419066, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 2,5-Difluoroaniline | HCID 67775 | — |
| Reactant | Potassium ethylxanthate | HCID 2735045 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178419066 | HCID 178419066 | 67% |
Reaction Conditions
| Temperature | 120 °C |
|---|
Reaction Steps
A mixture of 2,5-difluoro-phenylamine (129 mg, 1 mmol) and potassium o-ethyl dithiocarbonate (352 mg, 2.2 mmol) in DMF (5 mL) was heated to 120° C. for 15 min in microwave. The reaction mixture was cooled, diluted with 10 mL of ice water, and acidified with 3 mL of HCl solution (1 mol/L). Then the mixture was extracted with EtOAc (3×50 mL), washed with brine and dried over Na2SO4. The dried organic layers were concentrated to give 5-fluorobenzo[d]thiazole-2-thiol (120 mg, 0.67 mmol, 67%). ESI-MS (M+1): 185 calc. for C7H4FN4S2 184.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08952037B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-12e26a863ec145908fe04a17fb31f3d1 |
| Source note | uspto-grants-2015_02 |