反应详情

Compound 26 (60 mg, 0.149 mmol) was refluxed in phosphorous oxychloride (2 mL) for 1 h. The reaction mixture was concentrated and diluted with ice-cold water, brought to pH ˜8 with slow addition of saturated NaHCO3 and extracted with dichloromethane. The organic layer was dried over Na2SO4 and concentrated to afford 27, which was used in Step 3 without purification.

1. concentrationThe reaction mixture was concentrated
2. additiondiluted with ice-cold water
3. additionbrought to pH ˜8 with slow addition of saturated NaHCO3
4. extractionextracted with dichloromethane
5. dry with materialThe organic layer was dried over Na2SO4
6. concentrationconcentrated