8-methoxy-2H-chromene → HCID 13758736、化合物

HRID 581070ノート

反応式

HRID 581070 の反応式
[CH3:1][O:2][C:3]1[C:12]2[O:11][CH2:10][CH:9]=[CH:8][C:7]=2[CH:6]=[CH:5][CH:4]=1.[H][H]>C(O)(=O)C.[Pd]>[CH3:1][O:2][C:3]1[C:12]2[O:11][CH2:10][CH2:9][CH2:8][C:7]=2[CH:6]=[CH:5][CH:4]=1

参加物

5

反応物 2

HCID 123719428-methoxy-2H-chromeneHCID 178418361HCID 178418361、化合物

生成物 1

HCID 13758736HCID 13758736、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒

実験手順

The compound obtained in Step B (1 g:6.84 mmol) dissolved in glacial acetic acid (10 ml) is poured into the reactor of a Paar apparatus. 10% palladium on carbon (10% by weight; 100 mg), acting as catalyst, is added. The whole is then subjected to a hydrogen pressure of 45 psi for 12 hours at room temperature. After filtration, the solvent is removed under reduced pressure and then extraction is carried out with dichloromethane. The recovered organic phase, dried over magnesium sulphate, is purified after concentration over a silica column eluted with pure dichloromethane. The title product is obtained pure in the form of a yellow oil.

後処理

  1. additionis poured into the reactor of a Paar apparatus
  2. additionis added
  3. filtrationAfter filtration
  4. customthe solvent is removed under reduced pressure
  5. extractionextraction
  6. dry with materialThe recovered organic phase, dried over magnesium sulphate
  7. customis purified
  8. concentrationafter concentration over a silica column
  9. washeluted with pure dichloromethane

出典と根拠

ORDレコード
ord-6eb18eefd2fe4e75b69526204d65328d
出典データセット
uspto-grants-1999_07
特許番号
US05919814

反応ノート

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