반응 #2380

ord-a95cb73bbffa41a19d32814251cb5b39

반응 방정식

Cc1ccc(-c2c(NS(=O)(=O)c3ccc(C(C)(C)C)cc3)ncnc2OCCOc2ccc(OCc3ccccc3)cc2)cc1
4-tert-butyl-N-{6-[2-(4-benzyloxyphenoxy)ethoxy]-5-(4-methylphenyl)pyrimidin-4-yl}benzensulfonamide
Cc1ccc(-c2c(NS(=O)(=O)c3ccc(C(C)(C)C)cc3)ncnc2OCCOc2ccc(O)cc2)cc1
4-tert-butyl-N-{6-[2-(4-hydroxyphenoxy)ethoxy]-5-(4-methylphenyl)pyrimidin-4-yl}benzenesulfonamide
수율 97.9%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타is subjected to catalytic hydrogenation at room temperature under hydrogen atmosphere
  2. 2
    기타for 24 hours
  3. 3
    기타The catalyst is removed by filtration
  4. 4
    농축the filtrate is concentrated
  5. 5
    기타The residue is crystallized from ethyl acetate/diisopropyl ether

실험 절차

A mixture of 4-tert-butyl-N-{6-[2-(4-benzyloxyphenoxy)ethoxy]-5-(4-methylphenyl)pyrimidin-4-yl}benzensulfonamide (3.95 g), 10% palladium-carbon (1.5 g) and ethanol-tetrahydrofuran (80 ml-80 ml) is subjected to catalytic hydrogenation at room temperature under hydrogen atmosphere (1 atm) for 24 hours. The catalyst is removed by filtration, and the filtrate is concentrated. The residue is crystallized from ethyl acetate/diisopropyl ether to give 4-tert-butyl-N-{6-[2-(4-hydroxyphenoxy)ethoxy]-5-(4-methylphenyl)pyrimidin-4-yl}benzenesulfonamide (3.31 g).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05728706uspto-grants-1998_03