反应详情

To a round bottom flask, (E)-N′-(3-(1H-indol-3-yl)acryloyl)-N′-isopropylbenzohydrazide (60 mg, 0.17 mmol, 1.0 equivalent), K2CO3 (71.6 mg, 0.51 mmol, 3.0 equivalent), and DMAP (cat, 0.12 equivalent) were introduced and dissolved in DMF, after which Piv-Cl (0.04 ml, 0.34 mmol, 2.0 equivalent) was introduced. After stirring at room temperature for 24 hr, the reaction mixture was diluted with EtOAc, washed with water and brine, dried with anhydrous MgSO4, filtered, and concentrated under reduced pressure. The residue was separated through silica gel chromatography (n-hexane:EtOAc:methanol=7:3:1) and dried so that solid form of (E)-N′-(3-(1-acetyl-1H-indol-3-yl)acryloyl)-N′-isopropylbenzohydrazide was obtained. (10.3 mg, 14%).

1. washwashed with water and brine
2. dry with materialdried with anhydrous MgSO4
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. customThe residue was separated through silica gel chromatography (n-hexane:EtOAc:methanol=7:3:1)
6. dry with materialdried so that solid form of (E)-N′-(3-(1-acetyl-1H-indol-3-yl)acryloyl)-N′-isopropylbenzohydrazide
7. customwas obtained