反应详情

温度

30 °C

Under anhydrous conditions, the compound obtained in Step B (1 g; 5.52 mmol) is dissolved in an acetonitrile/dichloromethane mixture (4/6). Sodium hydroxide (4 eq.; 22.1 mmol; 883 mg) that has been ground beforehand, dibromoethane (4 eq.; 22.1 mmol; 1.96 mmol) and Aliquat 336 (catalytic amount) are added to the solution. The whole is stirred for 24 hours at 30° C., under argon, and then 220 mg (1 eq.) of sodium hydroxide are added to terminate the reaction. The solution is filtered through fritted glass, and the brown solid is rinsed with ether. The red filtrate is recovered, and the solvents are removed under reduced pressure. The residue obtained is purified by flash chromatography on silica gel (eluant: PE/AcOEt (1/1)). The title product is obtained in the form of a red solid.

1. customto terminate
2. customthe reaction
3. filtrationThe solution is filtered through fritted glass
4. washthe brown solid is rinsed with ether
5. customThe red filtrate is recovered
6. customthe solvents are removed under reduced pressure
7. customThe residue obtained
8. customis purified by flash chromatography on silica gel (eluant: PE/AcOEt (1/1))