반응 #2391

반응 방정식

4-tert-butyl-N-{6-[2-(5-methylsulfinylpyrimidin-2-yloxy)ethoxy]-5-(4-methylphenyl)pyrimidin-4-yl}benzenesulfonamide

→

4-tert-butyl-N-{6-[2-(5-mercaptopyrimidin-2-yloxy)ethoxy]-5-(4-methylphenyl)pyrimidin-4-yl}benzenesulfonamide

수율 118.4%

용매

trifluoroacetic anhydride

methylene chloride

반응 조건

후처리

1. 1
   기타the mixture is evaporated
2. 2
   기타to remove the solvent
3. 3
   workup.DISSOLUTIONThe residue is dissolved in methanol/triethylamine (1:1) (20 ml)
4. 4
   농축concentrated to dryness under reduced pressure
5. 5
   workup.DISSOLUTIONThe residue is dissolved in chloroform
6. 6
   세척washed with saturated aqueous ammonium chloride solution and brine
7. 7
   건조dried over sodium sulfate
8. 8
   여과filtered
9. 9
   농축The filtrate is concentrated under reduced pressure

실험 절차

A solution of 4-tert-butyl-N-{6-[2-(5-methylsulfinylpyrimidin-2-yloxy)ethoxy]-5-(4-methylphenyl)pyrimidin-4-yl}benzenesulfonamide (471 mg) in trifluoroacetic anhydride (5 ml) and methylene chloride (5 ml) is refluxed for 30 minutes, and the mixture is evaporated to remove the solvent. The residue is dissolved in methanol/triethylamine (1:1) (20 ml), and concentrated to dryness under reduced pressure. The residue is dissolved in chloroform, washed with saturated aqueous ammonium chloride solution and brine, dried over sodium sulfate, and filtered. The filtrate is concentrated under reduced pressure to give 4-tert-butyl-N-{6-[2-(5-mercaptopyrimidin-2-yloxy)ethoxy]-5-(4-methylphenyl)pyrimidin-4-yl}benzenesulfonamide as pale yellow foam (529 mg).

출처