Water → HCID 68776951, Verbindung

A mixed solution of bis(2,2,2-trichloroethyl) 1H-indazol-3-ylimidodicarbonate (295 mg, 0.61 mmol), 1-(3-phenyl-1,2,4-thiadiazol-5-yl)piperazine (300 mg, 1.22 mmol) and diisopropylethylamine (0.106 ml, 0.610 mmol) in dimethyl sulfoxide (2.5 ml) was stirred at 80° C. for 5 hours. Water was poured to the reaction mixture, and the resulting solution was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (100% ethyl acetate, followed by ethyl acetate:methanol=1:1) and recrystallized from a mixed solvent of hexane and tetrahydrofuran to give 30.2 mg (12.2%) of the desired product as a solid.

1. extractionthe resulting solution was extracted with ethyl acetate
2. washThe extract was washed with water
3. dry with materialdried over anhydrous magnesium sulfate
4. distillationthe solvent was distilled off under reduced pressure
5. customThe residue was purified by silica gel column chromatography (100% ethyl acetate, followed by ethyl acetate:methanol=1:1)
6. customrecrystallized from a mixed solvent of hexane and tetrahydrofuran

ORD-Eintrag

ord-50f4208900f44522bc1f07738ae4758a

Quelldatensatz

uspto-grants-2010_12

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07851473B2