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Water → HCID 19688467, 화합물

HRID 1093434
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HRID 1093434 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][C:3]=1[CH2:9][CH2:10][CH2:11]O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Br:32]N1C(=O)CCC1=O.O>C(Cl)Cl>[Br:32][CH2:11][CH2:10][CH2:9][C:3]1[CH:4]=[C:5]([CH3:8])[CH:6]=[CH:7][C:2]=1[CH3:1]
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참가 물질

6

반응물 4

HCID 962WaterHCID 11776TriphenylphosphineHCID 67184N-bromobutanimideHCID 190752692,5-Dimethylbenzenepropanol

생성물 1

HCID 19688467HCID 19688467, 화합물수율 86.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Compound 62-2 (1.64 g) was dissolved in methylene chloride (33 ml), triphenylphosphine (2.90 g) and N-bromosuccinimide (1.95 g) were added under ice-cooling, and the mixture was stirred under ice-cooling for 3.5 hr. Water was added to the reaction mixture, and the mixture was extracted with methylene chloride and washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. Diethyl ether was added, and the precipitated triphenylphosphine oxide was filtered off. The concentrate of the filtrate was purified by silica gel column chromatography (hexane alone) to give the object product (1.97 g) as a colorless oil.

후처리

  1. temperaturecooling
  2. temperaturecooling for 3.5 hr
  3. extractionthe mixture was extracted with methylene chloride
  4. washwashed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. additionDiethyl ether was added
  8. filtrationthe precipitated triphenylphosphine oxide was filtered off
  9. concentrationThe concentrate of the filtrate
  10. customwas purified by silica gel column chromatography (hexane alone)

출처 및 근거

ORD 기록
ord-6bfb7aea23ae4baaaf7dd43cd6cce673
출처 데이터셋
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08129361B2

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