HCID 86600789, compound → HCID 69047710, compound

Participants

Reaction Conditions

Reaction Steps

Compound 39d (0.9 g; 2.4 mmol) is dissolved in a mixture of 1,4-dioxane/water (1:1; 15 ml). LiOH monohydrate (0.302 g; 7.2 mmol) is added as a solid and the mixture is stirred for 18 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: 0.7 g (84.1%), ESI-MS: m/z=345 [M−H]−, Cl-pattern

Provenance & Evidence