反応 #1985941

反応方程式

bromine

4-acetoxy-3-methoxybenzaldehyde

sodium acetate

iodine

→

desired product

4-Acetoxy-6-bromo-3-methoxybenzaldehyde

溶媒

water

acetic acid

反応条件

後処理

1. 1
   workup.STIRRINGstirred at room temperature for 3 days
2. 2
   ろ過filtered
3. 3
   workup.DISSOLUTIONThe solid is dissolved in toluene
4. 4
   洗浄the solution washed with brine
5. 5
   乾燥dried over magnesium sulfate
6. 6
   ろ過filtered
7. 7
   濃縮concentrated in vacuo
8. 8
   その他The residue is recrystallized twice from hexanes

実験手順

To a mixture of 4-acetoxy-3-methoxybenzaldehyde (75.7 g), anhydrous sodium acetate (76 g) and iodine (0.8 g) in acetic acid (300 ml) is added bromine (21 ml). The mixture is warmed to 45° C. for about 1 hour, then stirred stirred at room temperature for 3 days, poured into water (700 ml) and filtered. The solid is dissolved in toluene and the solution washed with brine, dried over magnesium sulfate, filtered and concentrated in vacuo. The residue is recrystallized twice from hexanes to give the desired product.

出典