1H-1,2,4-Triazole, 5-bromo-1-methyl- → 5-(7-[1,3]Dioxan-2-yl-benzofuran-5-yl)-1-methyl-1H[1,2,4]triazole

A mixture of tributyl-(7-[1,3]dioxan-2-ylbenzofuran-5-yl)stannane (839 mg), 5-bromo-1-methyl-1H-[1,2,4]triazole (396 mg), bis(triphenylphosphine)palladium (II) chloride (59 mg) in dry toluene (10 ml) was heated at reflux for 42 h. The cooled solution was then filtered through Hyflo and the filtrate washed with 10% potassium fluoride solution (30 ml). The organic layer was washed with brine (30 ml), dried, and evaporated in vacuo to give a yellow oil. The crude material was purified by FCC eluting with hexane:ethyl acetate (1:1→1:3) to give the title compound as a yellow oil (171 mg,).

1. temperaturewas heated
2. temperatureat reflux for 42 h
3. filtrationThe cooled solution was then filtered through Hyflo
4. washthe filtrate washed with 10% potassium fluoride solution (30 ml)
5. washThe organic layer was washed with brine (30 ml)
6. customdried
7. customevaporated in vacuo
8. customto give a yellow oil
9. customThe crude material was purified by FCC
10. washeluting with hexane:ethyl acetate (1:1→1:3)

ORD-Eintrag

ord-8ae8b9a041e5485690cd599915b31973

Quelldatensatz

uspto-grants-1999_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05935972