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

HRID 1446396노트

반응식

HRID 1446396 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

반응물 3

HCID 3283Diethyl EtherHCID 12391212HCID 12391212, 화합물HCID 178418287HCID 178418287, 화합물

생성물 1

HCID 222703593-(2,4-Dichlorophenyl)-2-(4-chlorophenyl)propanal

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 3-(2,4-dichlorophenyl)-2-(4-chlorophenyl)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-583c2463d86546358b10e32156979962
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07667053B2

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