HCID 86600788, compound → HCID 69048291, compound

Participants

Reaction Conditions

Reaction Steps

Compound 28d (3.7 g; 8 mmol) is dissolved in a mixture of 1,4-dioxane/water (1:1; 30 ml). LiOH monohydrate (1.03 g; 25 mmol) is added to the mixture and complete saponification is obtained after stirring for 24 h at 25° C. The mixture is evaporated to dryness and dissolved in ethyl acetate and the product is extracted with saturated aqueous Na2CO3 solution. The aqueous phase is cooled to 10° C. and acidified with 25% aqueous HCl solution until pH=1. The product is extracted several times with ethylacetate (3×100 ml). The combined organic phases are washed with brine and dried over Na2SO4. After filtration the organic phase is evaporated to dryness. Yield: 1.57 g (45.2%), ESI-MS: m/z=422 [M−H]−

Provenance & Evidence