反应详情

According to Scheme 3 Method A: The title compound was prepared according to Example 2 Step 2, from 1-(4-chlorobenzyl)-5-bromopyridin-2(1H)-one (1 eq, 0.67 mmol, 0.20 g, Example 2 Step 1) and 2-(4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)acetic acid (1.5 eq, 1.00 mmol, 0.26 g). Reaction conditions: 4.5 hours at 90° C. The reaction mixture was made acidic then extracted with AcOEt. The organic layer washed with brine, dried over Na2SO4, filtered and concentrated. The residue was purified by chromatography over silicagel (AIT Flashsmart prepacked column 25 g SiO2, AcOEt/MeOH 95/5), yielding the title compound (0.24 g, 100%) as a white solid. LC (XTerra RP18, 3.5 μm, 3.0×50 mm Column): RT=3.53 min; MS m/z (CI) [MH]+=354, 356.

1. customThe title compound was prepared
2. customReaction conditions
3. custom4.5 hours
4. customat 90° C
5. extractionThe reaction mixture was made acidic then extracted with AcOEt
6. washThe organic layer washed with brine
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. concentrationconcentrated
10. customThe residue was purified by chromatography over silicagel (AIT Flashsmart prepacked column 25 g SiO2, AcOEt/MeOH 95/5)