反应详情

A solution of 563 (460 mg, 1.78 mmol) and TFA (5 ml) in DCM (20 ml) was stirred at rt for 5 h. The reaction mixture was concentrated (azeotropes with DCM), diluted with water, stirred for 10 min. The pH was adjusted to around 10 with 1N NaOH, and the alkaline solution was extracted with DCM. The organic extract was dried over anhydrous magnesium sulfate, filtered, concentrated under high vacuum to afford the desired product 564 (170 mg, 1.07 mmol, 60% yield) as a dark orange sticky solid. The crude product was used in the next step without any further purification. MS (m/z): 159.13 (M+H).

1. concentrationThe reaction mixture was concentrated (azeotropes with DCM)
2. additiondiluted with water
3. extractionthe alkaline solution was extracted with DCM
4. extractionThe organic extract
5. dry with materialwas dried over anhydrous magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated under high vacuum