反応 #1447095

反応方程式

Phosphorus oxychloride

tin(IV) chloride

N-(4-bromo-3-methoxy-phenyl)-acetamide

4-ethylbenzoic acid

→

N-[4-Bromo-2-(4-ethyl-benzoyl)-5-methoxy-phenyl]-acetamide

溶媒

dichloromethane

1,2-dichloroethane

反応条件

後処理

1. 1
   その他maintains below 35° C
2. 2
   温度The resulting mixture is heated
3. 3
   温度at reflux temperature overnight
4. 4
   workup.ADDITIONpoured
5. 5
   その他onto crushed ice
6. 6
   その他the organic phase is separated
7. 7
   洗浄washed with 10% NaOH in water and water
8. 8
   乾燥The organic phase is dried (sodium sulphate)
9. 9
   その他the solvent is removed
10. 10
    その他the residue is triturated with methanol
11. 11
    その他to give the product

実験手順

Phosphorus oxychloride (17 mL) and tin(IV) chloride (5 mL) are successively added to a suspension of N-(4-bromo-3-methoxy-phenyl)-acetamide (5.0 g) and 4-ethylbenzoic acid (4.4 g) in 1,2-dichloroethane at such a rate that the temperature maintains below 35° C. The resulting mixture is heated at reflux temperature overnight. Then, the mixture is diluted with dichloromethane and poured onto crushed ice. After stirring the aqueous mixture for 30 min, the organic phase is separated and washed with 10% NaOH in water and water. The organic phase is dried (sodium sulphate), the solvent is removed and the residue is triturated with methanol to give the product.

出典