反应详情

温度

90 °C

A solution obtained beforehand by adding thiourea (52 mg, WAKO) to 1 M sulfuric acid (5 ml) and mixing them was added with a solution of Intermediate 76 (101 mg) in acetonitrile (5 ml), and stirred at 90° C. for 20 hours. The reaction mixture was poured into water (20 ml), neutralized by addition of 1 N aqueous sodium hydroxide under ice cooling, and then extracted with ethyl acetate (80 ml×3). The organic layer was washed with saturated brine and dried, and then the solvent was evaporated under reduced pressure. The residue was purified by column chromatography (Quad, methylene chloride:ethanol=30:1) to obtain the title compound (Compound No. V-91, 46 mg).

1. customA solution obtained
2. additionmixing them
3. extractionextracted with ethyl acetate (80 ml×3)
4. washThe organic layer was washed with saturated brine
5. customdried
6. customthe solvent was evaporated under reduced pressure
7. customThe residue was purified by column chromatography (Quad, methylene chloride:ethanol=30:1)