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

HRID 359216

反応式

HRID 359216 の反応式
[CH:1]1[C:2]2[CH:19]=[CH:18][C:17]3[C:16]4[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=4[CH:10]=[CH:9][C:8]=3[C:3]=2[O:4][C:5]=1[CH2:6][OH:7].[Mn]([O-])([O-])(=O)=O.[Ba+2]>C(Cl)Cl>[CH:1]1[C:2]2[CH:19]=[CH:18][C:17]3[C:16]4[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=4[CH:10]=[CH:9][C:8]=3[C:3]=2[O:4][C:5]=1[CH:6]=[O:7]

参加物

4

反応物 2

HCID 3084030Barium manganateHCID 14770239Phenanthro[1,2-b]furan-2-methanol

生成物 1

HCID 14770240Phenanthro[1,2-b]furan-2-carbaldehyde収率 91%

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 phenanthro[1,2-b]furan-2-methanol (14A, 5.84 g, 23.5 mmol), barium manganate (Aldrich, 12.06 g, 47 mmol) and dry CH2Cl2 (400 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 baseline material. The solvent was then removed by rotary evaporation and the crude material recrystallized using CH2Cl2 /hexane to give after drying 5.17 g (91% yield) of phenanthro[1,2-b]furan-2-carbaldehyde, mp 169° , (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 baseline material
  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-004e2a8b102a4efdb02909daee17cee3
出典データセット
uspto-grants-1991_03
特許番号
US04999369

関連ノート

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