반응 #2369

반응 방정식

4-tert-butyl-N-[6-{2-(6-chloropyridazin-3-yloxy)ethoxy}-5-(3-methoxyphenoxy)pyrimidin-4-yl]benzenesulfonamide

triethylamine

methanol

→

4-tert-butyl-N-[5-(3-methoxyphenoxy)-6-{2-(pyridazin-3-yloxy)ethoxy}pyrimidin-4-yl]benzenesulfonamide

수율 78.6%

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   여과the mixture is filtered
2. 2
   기타to remove the catalyst
3. 3
   농축The filtrate is concentrated to dryness under reduced pressure
4. 4
   workup.ADDITIONThe residue is treated with aqueous citric acid solution
5. 5
   추출extracted with chloroform
6. 6
   세척The extract is washed
7. 7
   기타dried
8. 8
   기타evaporated
9. 9
   기타to remove the solvent
10. 10
    기타The residue is recrystallized from ethyl acetate/diisopropyl ether

실험 절차

A mixture of 4-tert-butyl-N-[6-{2-(6-chloropyridazin-3-yloxy)ethoxy}-5-(3-methoxyphenoxy)pyrimidin-4-yl]benzenesulfonamide (150 mg), 10% palladium-carbon (30 mg), triethylamine (52 mg), methanol (8 ml) and tetrahydrofuran (6 ml) is stirred at room temperature for five hours under hydrogen atmosphere (1 atm), and the mixture is filtered to remove the catalyst. The filtrate is concentrated to dryness under reduced pressure. The residue is treated with aqueous citric acid solution, and extracted with chloroform. The extract is washed, dried and evaporated to remove the solvent. The residue is recrystallized from ethyl acetate/diisopropyl ether to give 4-tert-butyl-N-[5-(3-methoxyphenoxy)-6-{2-(pyridazin-3-yloxy)ethoxy}pyrimidin-4-yl]benzenesulfonamide (111 mg) as crystals.

출처