反应详情

The compound (50 mg, 0.12 mmol) obtained in Step 5 of Example 1 was dissolved in pyridine (1.5 mL), and cis-3-chloroacrylic acid (18 mg, 0.17 mmol) and N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloric acid salt (44 mg, 0.23 mmol) were added thereto, followed by stirring at room temperature for 1 hour. After the reaction was complete, the reaction mixture was diluted with a mixed solvent (chloroform:2-propanol=3:1 (volume ratio)) and washed with sat. brine. The organic layer was dried with anhydrous sodium sulfate and then filtered and distilled under a reduced pressure. The residue was separated by column chromatography (dichloromethane:methanol=6:1 (volume ratio)) to obtain the title compound (yield: 15 mg, 24%).

1. washwashed with sat. brine
2. dry with materialThe organic layer was dried with anhydrous sodium sulfate
3. filtrationfiltered
4. distillationdistilled under a reduced pressure
5. customThe residue was separated by column chromatography (dichloromethane:methanol=6:1 (volume ratio))