Hydrochloric Acid → HCID 19973110, Verbindung

To 10 ml of dried tetrahydrofuran were added 0.36 g of N-(2-hydroxyethyl)-3-(2,4-difluorophenyl)-2,2-difluoro-3-hydroxy-4-(1H-1,2,4-triazol-1-yl)butanamide, 0.39 g of triphenylphosphine and 0.26 g of diethyl azodicarboxylate. The resulting mixture was subjected to reaction at 20°-25° C. for 12 hours. The reaction mixture was introduced into a mixed solvent consisting of 20 ml of ethyl acetate and 10 ml of water. The resulting solution was adjusted to pH 2.0 with 6N hydrochloric acid. The organic layer was separated, washed with a saturated aqueous sodium chloride solution, and then dried over anhydrous magnesium sulfate. Thereafter, the solvent was removed by distillation under reduced pressure. The residue thus obtained was purified by a column chromatography (eluant: toluene/ethyl acetate=10/1) to obtain 0.13 g of 1-aziridinylcarbonyl-2-(2,4-difluorophenyl)-1,1-difluoro-2-hydroxy-3-(1H-1,2,4-triazol-1-yl)propane.

1. customThe resulting mixture was subjected to reaction at 20°-25° C. for 12 hours
2. additionThe reaction mixture was introduced into a mixed solvent
3. customThe organic layer was separated
4. washwashed with a saturated aqueous sodium chloride solution
5. dry with materialdried over anhydrous magnesium sulfate
6. customThereafter, the solvent was removed by distillation under reduced pressure
7. customThe residue thus obtained
8. customwas purified by a column chromatography (eluant: toluene/ethyl acetate=10/1)

ORD-Eintrag

ord-a8bc612a239f4b7085ad6d0ebf161951

Quelldatensatz

uspto-grants-1997_02

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05605921