反应 #1994243
ord-d6d60343bd5e4faba8cf8df11ffe0555
反应方程式
反应条件
后处理
- 1workup.STIRRINGAfter stirring for 3.5 hrs
- 2其他freeze-dried for 16 hrs
- 3萃取The organic residue is then extracted with CH2Cl2 (40 mL)
- 4过滤filtered
- 5浓缩concentrated under reduced pressure
- 6其他to provide a brown viscous liquid
- 7其他Purification
实验过程
In a round bottom flask, Compound 5 (2.2 g, 13×10−3 mol) is treated with a solution of K2CO3 (5.6 g, 40×10−3 mol, in 20 mL of water), with magnetic stirring at room temperature. The progress of the reaction is followed by TLC (eluent: ethyl acetate/methanol, 98/2). After stirring for 3.5 hrs, the reaction is complete. The reaction mixture is neutralized (pH=7) by adding 1N hydrochloric acid and then freeze-dried for 16 hrs. The organic residue is then extracted with CH2Cl2 (40 mL), filtered and then concentrated under reduced pressure to provide a brown viscous liquid. Purification was carried out on a silica gel column (eluent: ethyl acetate/methanol, 98/2). Compound 6 is obtained after such purification as a white powder.