反应详情

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).

1. customthe mixture is evaporated
2. customto remove the solvent
3. dissolutionThe residue is dissolved in methanol/triethylamine (1:1) (20 ml)
4. concentrationconcentrated to dryness under reduced pressure
5. dissolutionThe residue is dissolved in chloroform
6. washwashed with saturated aqueous ammonium chloride solution and brine
7. dry with materialdried over sodium sulfate
8. filtrationfiltered
9. concentrationThe filtrate is concentrated under reduced pressure