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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
ノート
印刷プレビュー

反応式

HRID 1584782 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 1401211H-1,2,4-Triazole, 5-bromo-1-methyl-HCID 21220869HCID 21220869、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 6102075Dichlorobis(triphenylphosphine)palladium触媒HCID 1140Toluene溶媒

実験手順

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,).

後処理

  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)

出典と根拠

ORDレコード
ord-8ae8b9a041e5485690cd599915b31973
出典データセット
uspto-grants-1999_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05935972

反応ノート

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