تفاعل #1447095

معادلة التفاعل

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

المذيبات

dichloromethane

1,2-dichloroethane

ظروف التفاعل

المعالجة

1. 1
   أخرىmaintains below 35° C
2. 2
   درجة الحرارةThe resulting mixture is heated
3. 3
   درجة الحرارةat reflux temperature overnight
4. 4
   workup.ADDITIONpoured
5. 5
   أخرىonto crushed ice
6. 6
   أخرىthe organic phase is separated
7. 7
   غسيلwashed with 10% NaOH in water and water
8. 8
   تجفيفThe organic phase is dried (sodium sulphate)
9. 9
   أخرىthe solvent is removed
10. 10
    أخرىthe residue is triturated with methanol
11. 11
    أخرىto give the product

الإجراء التجريبي

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.

المصدر