Hydrochloric Acid → 2-Amino-4-fluorobenzene-1-thiol

Temperatur

129 °C

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.

1. temperatureThe solution was cooled to 0° C.
2. extractionThe mixture was extracted with EtOAc (2×50 ml)
3. washThe organic layer was washed with brine
4. dry with materialdried with Na2SO4
5. concentrationconcentrated in vacuo
6. customThe crude residue (1.01 g, 98%) was used directly in the next step without purification

ORD-Eintrag

ord-9973628e03304ad8a572efcad5813af5

Quelldatensatz

uspto-grants-2014_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08791161B2