HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 2-Amino-4-fluorobenzene-1-thiol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 5-Fluoro-2-methylbenzothiazole | HCID 597437 | — |
| Solvent | Ethylene Glycol | HCID 174 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Product | 2-Amino-4-fluorobenzene-1-thiol | HCID 11105480 | — |
Reaction Conditions
| Temperature | 129 °C |
|---|
Reaction Steps
A solution of 5-fluoro-2-methylbenzo[d]thiazole (1.2 g, 7.18 mmol) in ethylene glycol and NaOH (5N, 2 ml) was degassed under N2 for 10 min, then refluxed at 129° C. for 3 hours. The solution was cooled to 0° C. and then acidified to pH 3˜4 using c. HCl. The mixture was extracted with EtOAc (2×50 ml). The organic layer was washed with brine and dried with Na2SO4 and concentrated in vacuo. The crude residue (1.01 g, 98%) was used directly in the next step without purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08791161B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-9973628e03304ad8a572efcad5813af5 |
| Source note | uspto-grants-2014_07 |