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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

HRID 1584782
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HRID 1584782 반응식
C([Sn](CCCC)(CCCC)[C:6]1[CH:7]=[C:8]([CH:15]2[O:20][CH2:19][CH2:18][CH2:17][O:16]2)[C:9]2[O:13][CH:12]=[CH:11][C:10]=2[CH:14]=1)CCC.Br[C:30]1[N:34]([CH3:35])[N:33]=[CH:32][N:31]=1>C1(C)C=CC=CC=1.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.Cl[Pd]Cl>[O:20]1[CH2:19][CH2:18][CH2:17][O:16][CH:15]1[C:8]1[C:9]2[O:13][CH:12]=[CH:11][C:10]=2[CH:14]=[C:6]([C:30]2[N:34]([CH3:35])[N:33]=[CH:32][N:31]=2)[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 1401211H-1,2,4-Triazole, 5-bromo-1-methyl-HCID 21220869HCID 21220869, 화합물

생성물 1

HCID 212208495-(7-[1,3]Dioxan-2-yl-benzofuran-5-yl)-1-methyl-1H[1,2,4]triazole수율 35.2%

시약·촉매·용매 2

HCID 6102075Dichlorobis(triphenylphosphine)palladium촉매HCID 1140Toluene용매

실험 절차

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,).

후처리

  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)

출처 및 근거

ORD 기록
ord-8ae8b9a041e5485690cd599915b31973
출처 데이터셋
uspto-grants-1999_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05935972

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