Potassium Phosphate, Tribasic → HCID 66743216, compound

Participants

Reaction Conditions

Reaction Steps

This reaction was carried out under similar conditions to those described above in step 7 of preparation of Example 6. (1R,5S)-tert-butyl 8-(6-(6-chloro-2-methyl-3-oxo-2,3-dihydropyridazin-4-ylamino)pyridin-3-yl)-3,8-diazabicyclo[3.2.1]octane-3-carboxylate (100 mg, 224 umol), 2-(6-tert-butyl-8-fluoro-1-oxophthalazin-2(1H)-yl)-6-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzyl acetate (114 mg, 224 umol), xPhos (10.7 mg, 22.4 umol) and potassium phosphate (119 mg, 559 umol) in 7 ml of Dioxane/water (9:1) was degassed with nitrogen for 10 minutes and bis(dibenzylideneacetone)palladium (0) (6.42, 11.2 umol) was added. The reaction mixture was heated to 100° C. for 2 hr. After work up, the product was purified by preparative HPLC on silica gel, using a gradient of 5% to 70% ethylacetate/hexane. This provided the desired product as a light yellow solid (105 mg 60.3%). (M+H)+=779 m/e.

Provenance & Evidence