反应详情

To a solution of 0.200 g (0.381 mmol) of the product of Example 65 dissolved in 1.5 mL of diethyl ether was added 0.837 mL (0.837 mmole) of 1.0M phosphorus tribromide in methylene chloride solution under nitrogen at 0° C. The reaction mixture was stirred at 0° C. for 2 hours when TLC analysis (80:15:1 CHCl3 -MeOH-NH4OH) indicated that the reaction was nearly complete. The reaction was quenched at 0° C. with water and then partitioned with EtOAc. The aqueous portion was separated and the EtOAc portion was washed with brine (2×10 mL). The EtOAc portion was then dried over MgSO4, filtered, evaporated to a residue, and then used in the next step of the reaction scheme.

1. customThe reaction was quenched at 0° C. with water
2. custompartitioned with EtOAc
3. customThe aqueous portion was separated
4. washthe EtOAc portion was washed with brine (2×10 mL)
5. dry with materialThe EtOAc portion was then dried over MgSO4
6. filtrationfiltered
7. customevaporated to a residue
8. customused in the next step of the reaction scheme