Hydrazine hydrate (1:1) → HCID 59442813, compound

Participants

Reaction Conditions

Reaction Steps

1,4-dioxa-8-azaspiro[4.5]decane (2.2 ml) is added to a solution of 1-(3,4-dichlorophenyl)-3,3-bis(methylthio)prop-2-en-1-one (2.0 g) in ethanol (70 ml) and heated to 80° C. over night. Hydrazine-hydrate (1 ml) is added to the reaction mixture and the mixture is stirred over night at 80° C. The solvent is removed under reduced pressure. The crude product is purified using reverse phase HPLC (Varian C18 Microsorb) eluting with a gradient of 10-100% acetonitrile in water containing 0.2% trifluoroacetic acid to give 8-(5-(3,4-dichlorophenyl)-1H-pyrazol-3-yl)-1,4-dioxa-8-azaspiro[4.5]decane (550 mg). m/z(+) 354/356/358 (M+H+).

Provenance & Evidence