反应详情

温度

75 °C

Excess sodium metal was added to a stirred solution of the product of step E (0.651 g, 1.85 mmol) in methanol (5.0 mL) at ambient temperature, and the resulting solution was heated to 75° C. After approximately 1 h, 5 M sodium hydroxide (3.0 mL) was added and the reaction mixture heated to 100° C. for an additional 1 h. After cooling to room temperature, the reaction mixture was acidified to pH 5 with 2 N hydrochloric acid and extracted three times with methylene chloride. The combined organic extracts were washed with brine, dried (MgSO4) and concentrated in vacuo. The crude product was used without further purification in the subsequent reaction.

1. temperaturethe reaction mixture heated to 100° C. for an additional 1 h
2. temperatureAfter cooling to room temperature
3. extractionextracted three times with methylene chloride
4. washThe combined organic extracts were washed with brine
5. dry with materialdried (MgSO4)
6. concentrationconcentrated in vacuo
7. customThe crude product was used without further purification in the subsequent reaction