반응 #1447095

반응 방정식

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

용매

dichloromethane

1,2-dichloroethane

반응 조건

후처리

1. 1
   기타maintains below 35° C
2. 2
   온도The resulting mixture is heated
3. 3
   온도at reflux temperature overnight
4. 4
   workup.ADDITIONpoured
5. 5
   기타onto crushed ice
6. 6
   기타the organic phase is separated
7. 7
   세척washed with 10% NaOH in water and water
8. 8
   건조The organic phase is dried (sodium sulphate)
9. 9
   기타the solvent is removed
10. 10
    기타the residue is triturated with methanol
11. 11
    기타to give the product

실험 절차

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.

출처