5-benzylidene-2,2-dimethyl-1,3-dioxane-4,6-dione

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: This compound was prepared by using procedures analogous to those described for the synthesis of Example 120, Step 2 starting from 5-benzylidene-2,2-dimethyl-1,3-dioxane-4,6-dione and potassium cyanide. This compound was prepared

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: This compound was prepared by using procedures analogous to those described for the synthesis of Example 120, Step 2 starting from 5-benzylidene-2,2-dimethyl-1,3-dioxane-4,6-dione and potassium cyanide. This compound was prepared

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: This compound was prepared by using procedures analogous to those described for the synthesis of Example 120, Step 1 starting from benzaldehyde and 2,2-dimethyl-1,3-dioxane-4,6-dione. This compound was prepared

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of copper (II) acetate monohydrate (20 mg, 0.10 mmol) in water (0.4 ml) was treated with sodium (L)-ascorbate (40 mg, 0.20 mmol), the mixture was stirred until the mixture was turned bright orange (3 min). Subsequently, (R,M)-3-{[4-(2-diphenylphosphanyl-7-methoxy-naphthalen-1-yl)-phthalazin-1-ylamino]-phenyl-methyl}-pentan-3-ol (1st diastereomer, 66.2 mg, 0.10 mmol) and phenylacetylene (0.55 ml, 5.0 mmol) were added, the resulting mixture was stirred for 10 min at 23° C., cooled to 0° C., stirred for 5 min and treated with 5-benzylidene-2,2-dimethyl-1,3-dioxane-4,6-dione (116 mg, 0.50 mmol). The reaction mixture was stirred vigorously at 0° C. for 66 hrs, diluted with dichloromethane (2 ml) and subjected directly to flash chromatography on silica gel (hexane/EtOAc 3:1→1:1) to give 110 mg of the pure title compound as a white solid. (yield: 64%) orange (3 min) the resulting mixture was stirred for 10 min at 23° C. stirred for 5 min The reaction mixture was stirred vigorously at 0° C. for 66 hrs

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: This compound was prepared by using procedures analogous to those described for the synthesis of Example 120, Step 2 starting from 5-benzylidene-2,2-dimethyl-1,3-dioxane-4,6-dione and potassium cyanide. This compound was prepared

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: This compound was prepared by using procedures analogous to those described for the synthesis of Example 120, Step 1 starting from benzaldehyde and 2,2-dimethyl-1,3-dioxane-4,6-dione. This compound was prepared