HCID 22734448、化合物 → HCID 22734278、化合物

HRID 2084792ノート

反応式

HRID 2084792 の反応式
[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Cl:23])[C:7]=1[CH2:8][CH:9]([C:11]1[C:20]2[O:19][CH2:18][CH2:17][O:16][C:15]=2[C:14]([O:21][CH3:22])=[CH:13][CH:12]=1)[OH:10].CC(C)=O.OS(O)(=O)=O.O=[Cr](=O)=O>CC(C)=O>[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Cl:23])[C:7]=1[CH2:8][C:9]([C:11]1[C:20]2[O:19][CH2:18][CH2:17][O:16][C:15]=2[C:14]([O:21][CH3:22])=[CH:13][CH:12]=1)=[O:10]

参加物

4

反応物 2

HCID 22734448HCID 22734448、化合物HCID 131709961Jones' reagent

生成物 1

HCID 22734278HCID 22734278、化合物収率 100.6%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

Compound 178a (3.0 g) obtained in Step A was dissolved in acetone (30 ml), mixed with Jones reagent (2.6 M) (4.9 ml), and stirred at room temperature for 2 hours. The reaction solution was concentrated under reduced pressure. The resulting residue was mixed with water and extracted with ethyl acetate. The organic layer was washed with a saturated aqueous sodium chloride solution, dried over magnesium sulfate anhydride, and evaporated under reduced pressure for removing the solvent. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=4/1) to give Compound 178 (3.0 g, 75%) as colorless crystals.

後処理

  1. concentrationThe reaction solution was concentrated under reduced pressure
  2. additionThe resulting residue was mixed with water
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with a saturated aqueous sodium chloride solution
  5. dry with materialdried over magnesium sulfate anhydride
  6. customevaporated under reduced pressure
  7. customfor removing the solvent
  8. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=4/1)

出典と根拠

ORDレコード
ord-26e2acd0a1a94d35a18918df7fb519f5
出典データセット
uspto-grants-2004_04
特許番号
US06716987B1

反応ノート

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