反应详情

温度

135 °C

A mixture of the product from Step B (200 mg, 0.3 mmol) in 1,4-dioxane (15 mL) and aqueous NaOH (2N, 15 mL) in a pressure bottle was heated overnight at 135° C. The mixture was then cooled to 0° C., neutralized with 2N aqueous HCl and evaporated to dryness. The crude product was suspended in MeOH, filtered, and the solid thoroughly washed with MeOH. The combined filtrate was concentrated, and the residue purified on a silica gel column (5×5 cm) using CH2Cl2/MeOH (40/1, 30/1 and 20/1) as eluent to give the desired compound (150 mg) as a colorless foam.

1. temperatureThe mixture was then cooled to 0° C.
2. customevaporated to dryness
3. filtrationfiltered
4. washthe solid thoroughly washed with MeOH
5. concentrationThe combined filtrate was concentrated
6. customthe residue purified on a silica gel column (5×5 cm)