Diethyl Ether → 3-(2,4-Dichlorophenyl)-2-(4-chlorophenyl)propanal

HRID 30362노트

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HRID 30362 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH2:9][CH:10]([C:13]1[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][CH:14]=1)[CH2:11][OH:12].[Cr](Cl)([O-])(=O)=O.[NH+]1C=CC=CC=1.CCOCC>C(Cl)Cl>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH2:9][CH:10]([C:13]1[CH:14]=[CH:15][C:16]([Cl:19])=[CH:17][CH:18]=1)[CH:11]=[O:12]

참가 물질

5

실험 절차

To a solution of 3-(2,4-dichlorophenyl)-2-(4-chorophenyl)propanol (Step B, 0.89 g, 2.8 mmol) in 20 mL CH2Cl2 was added crushed activated molecular sieves (4 g). After stirring at room temperature for 10 min, pyridinium chlorochromate (0.90 g, 4.2 mmol) was added. After stirring at room temperature for 1 h, CELITE diatomaceous earth (4 g) was added followed by 100 mL ether. The resulting mixture was filtered through a silica gel pad, which was washed with ether (2×50 mL). The filtrate was concentrated to dryness and azeotroped with toluene to give the title compound, which was used without further purification.

후처리

  1. customcrushed activated molecular sieves (4 g)
  2. stirringAfter stirring at room temperature for 1 h
  3. additionCELITE diatomaceous earth (4 g) was added
  4. filtrationThe resulting mixture was filtered through a silica gel pad, which
  5. washwas washed with ether (2×50 mL)
  6. concentrationThe filtrate was concentrated to dryness
  7. customazeotroped with toluene

출처 및 근거

ORD 기록
ord-5e33a3e3b9f64f40bdf888361e641c1b
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07423067B2

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