HCID 22734448, 화합물 → HCID 22734278, 화합물

HRID 1057906노트

반응식

HRID 1057906 반응식
[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]

참가 물질

4

반응물 2

HCID 22734448HCID 22734448, 화합물HCID 131709961Jones' reagent

생성물 1

HCID 22734278HCID 22734278, 화합물수율 100.6%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-a660f2639d67473f9f20935b879af2b9
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06514996B2

반응 노트

불러오는 중…