Thiourea → HCID 22648874, Verbindung

Temperatur

25 °C

Thiourea (79.8 mg, 1.05 mmol) was added to a solution of 2-bromo-1-(4-hydroxy-3-methylphenyl)ethanone (200 mg, 0.87 mmol) in 1,4-dioxane (15 mL). The reaction mixture was stirred at 25° C. for 24 h. The resulting suspension was filtered and the solid was washed with 1,4-dioxane and dried under reduced pressure. The solid was suspended in water (30 mL), pH 7 buffer solution (15 mL) was added and the mixture was extracted with EtOAc (3×50 mL). The combined organic layers were successively washed with water (20 mL) and brine (20 mL), dried (MgSO4), filtered and concentrated under reduced pressure. The residue was purified by flash chromatography (Hexane:EtOAc, 1:1) to give the title compound (180 mg, 100% yield).

1. filtrationThe resulting suspension was filtered
2. washthe solid was washed with 1,4-dioxane
3. customdried under reduced pressure
4. additionpH 7 buffer solution (15 mL) was added
5. extractionthe mixture was extracted with EtOAc (3×50 mL)
6. washThe combined organic layers were successively washed with water (20 mL) and brine (20 mL)
7. dry with materialdried (MgSO4)
8. filtrationfiltered
9. concentrationconcentrated under reduced pressure
10. customThe residue was purified by flash chromatography (Hexane:EtOAc, 1:1)

ORD-Eintrag

ord-96fcdb23cd8d45479baa46c5247ac730

Quelldatensatz

uspto-grants-2004_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06806265B2