反应详情

N′-Acetyl-5-{3-[(1S)-2-methoxy-1-methylethoxy]-5-[4-(methylsulfonyl)phenoxy]phenyl}-1H-pyrrole-2-carbohydrazide (58.1 mg, 0.116 mmol) synthesized in Example (22a) was dissolved in toluene (4 mL), 2,4-bis-(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane 2,4-disulfide (63.5 mg, 0.157 mmol) and pyridine (20 μL, 0.25 mmol) were added, and stirring was carried out at 90° C. for 5 hours under nitrogen atmosphere. The reaction solution was cooled to room temperature, water (20 mL) was added to the reaction solution, and extraction was carried out with ethyl acetate (20 mL). The organic layer was washed with saturated brine, and subsequently dried over sodium sulfate. The solvent was distilled off under reduced pressure, and the resulting residue was purified using silica gel column chromatography (elution solvent: ethyl acetate/hexane=40%-80%) to afford the desired compound (50.6 mg, yield 87%) as a pale yellow solid.

1. washThe organic layer was washed with saturated brine
2. dry with materialsubsequently dried over sodium sulfate
3. distillationThe solvent was distilled off under reduced pressure
4. customthe resulting residue was purified
5. washsilica gel column chromatography (elution solvent: ethyl acetate/hexane=40%-80%)