反应详情

温度

60 °C

The title compound of Example 20.1 (19.0 g, 67.0 mmol) was stirred in methanol (150 mL) and heated to 60° C. Methyl isothiocyanate (5.04 mL, 73.7 mmol) was then added via a syringe. After stirring for 40 minutes, a solution on NaOH (2.95 g, 73.7 mmol) in water (30 mL) was added and the reaction mixture was stirred at 60° C. overnight. The reaction mixture was cooled to room temperature and concentrated. The aqueous residue was neutralized, extracted with chloroform, and the organic layer dried over sodium sulfate and concentrated. The residue was purified by silica gel using ethyl acetate to give the product (24.0 g, 56%).

1. stirringthe reaction mixture was stirred at 60° C. overnight
2. temperatureThe reaction mixture was cooled to room temperature
3. concentrationconcentrated
4. extractionextracted with chloroform
5. dry with materialthe organic layer dried over sodium sulfate
6. concentrationconcentrated
7. customThe residue was purified by silica gel