반응 #1944813

반응 방정식

4-chloro-2-[2-(3,5-dimethylphenyl)-acetylamino]-5-iodo-benzoic acid methyl ester

allyltin

→

title compound

5-allyl-4-chloro-2-[2-(3,5-dimethylphenyl)-acetylamino]-benzoic acid methyl ester

반응 조건

후처리

1. 1
   온도the mixture was cooled
2. 2
   기타partitioned between ethyl acetate and water
3. 3
   세척the organic layer washed further with brine
4. 4
   건조Concentration of the dried (magnesium sulfate) organics
5. 5
   기타purification by flash chromatography on silica gel (hexane

실험 절차

To a suspension of 4-chloro-2-[2-(3,5-dimethylphenyl)-acetylamino]-5-iodo-benzoic acid methyl ester (2.39 g in 12 mL N,N-dimethylformamide) and 0.183 g bis(triphenylphosphine)palladium(II) chloride was added 2.02 mL allyltin and the mixture heated to 100° C. on an oil bath. After 2 hours, the mixture was cooled, partitioned between ethyl acetate and water and the organic layer washed further with brine. Concentration of the dried (magnesium sulfate) organics and purification by flash chromatography on silica gel (hexane:ethyl acetate, 95:5; then 90:10) gave the title compound (1.4 g).

출처