Barium manganate → Phenanthro[1,2-b]furan-2-carbaldehyde

HRID 728610

反応式

HRID 728610 の反応式
[O:1]1[C:5]([CH2:6][OH:7])=[CH:4][C:3]2[CH:8]=[CH:9][C:10]3[C:15]([C:2]1=2)=[CH:14][CH:13]=[CH:12][CH:11]=3.[Mn]([O-])([O-])(=O)=O.[Ba+2]>C(Cl)Cl>[CH:4]1[C:3]2[CH:8]=[CH:9][C:10]3[C:11]4[CH:4]=[CH:3][CH:2]=[CH:15][C:12]=4[CH:13]=[CH:14][C:15]=3[C:2]=2[O:1][C:5]=1[CH:6]=[O:7]

参加物

4

反応物 2

HCID 3084030Barium manganateHCID 14555902Naphtho[1,2-b]furan-2-methanol

生成物 1

HCID 14770240Phenanthro[1,2-b]furan-2-carbaldehyde収率 134.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a RB flask equipped with magnetic stirring bar, reflux condenser, N2 inlet line with bubbler was added naphtho[1,2-b]furan-2-methanol (11A, 4.8 g, 24.2 mmol), barium manganate (Aldrich, 12.4 g, 48 mmol) and dry CH2Cl2 (500 mL). The mixture was refluxed for 6 h, filtered and the resulting dark yellow solution filtered through a small plug of SiO2 to remove inorganic salts and polar materials. The solvent was then removed by rotary evaporation and the crude material recrystallized using CH2Cl2 /pentane to give after drying 4.02 g (84.7% yield) of phenanthro[1,2-b]furan-2-carbaldehyde, mp 123°, (C,H).

後処理

  1. customTo a RB flask equipped with magnetic stirring bar
  2. temperaturereflux condenser, N2 inlet line with bubbler
  3. temperatureThe mixture was refluxed for 6 h
  4. filtrationfiltered
  5. filtrationthe resulting dark yellow solution filtered through a small plug of SiO2
  6. customto remove inorganic salts and polar materials
  7. customThe solvent was then removed by rotary evaporation
  8. customthe crude material recrystallized
  9. customto give

出典と根拠

ORDレコード
ord-937a8bc3f7744cb58b1766da1b607321
出典データセット
uspto-grants-1991_09
特許番号
US05049581

関連ノート

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