反応 #76361
ord-d34af63acb464c238739b2729f02545b
反応方程式
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1温度cooled by an ice water bath
- 2抽出extracted with ethyl acetate (3×100 mL)
- 3洗浄The combined organic phases are washed with 100 mL portions of 5% NaHCO3 until no further gas evolution
- 4洗浄The organic phases are then washed with brine (100 mL)
- 5乾燥dried over anhydrous MgSO4
- 6濃縮concentrated in vacuo
- 7その他The mixture is purified by flash chromatography
実験手順
A solution of bromine (10 mmol) in 10 mL of acetic acid is added dropwise to a solution of ester 11 (10 mmol) in 10 mL of acetic acid cooled by an ice water bath. After the red color of the resulting mixture is discharged, the mixture is poured into saturated NaHCO3 (100 mL) and extracted with ethyl acetate (3×100 mL). The combined organic phases are washed with 100 mL portions of 5% NaHCO3 until no further gas evolution is apparent. The organic phases are then washed with brine (100 mL), dried over anhydrous MgSO4, and concentrated in vacuo. The mixture is purified by flash chromatography to give the product as a pale yellow solid.