Carbon Tetrachloride → HCID 59759003, 화합물

HRID 914484노트

반응식

HRID 914484 반응식
[CH3:1][O:2][CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11]O)=[CH:7][CH:6]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)(Cl)(Cl)[Cl:33]>>[Cl:33][CH2:11][C:8]1[CH:9]=[CH:10][C:5]([CH2:4][CH2:3][O:2][CH3:1])=[CH:6][CH:7]=1

참가 물질

4

반응물 3

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 59759121886531-77-7

생성물 1

HCID 59759003HCID 59759003, 화합물

실험 절차

[4-(2-Methoxyethyl)phenyl]methanol (415 mg) synthesized in Reference Example 42 was dissolved in carbon tetrachloride (8 mL), triphenylphosphine (720 mg) was added thereto, and the mixture was heated under reflux for 4 hr. The reaction mixture was concentrated under reduced pressure, the residue was dissolved in hexane, the insoluble material was filtered off, and the filtrate was evaporated under reduced pressure. The residue was purified by silica gel chromatography (elution solvent; hexane:ethyl acetate=20:1) to give the title compound (225 mg) as a colorless oil.

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 4 hr
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. dissolutionthe residue was dissolved in hexane
  5. filtrationthe insoluble material was filtered off
  6. customthe filtrate was evaporated under reduced pressure
  7. customThe residue was purified by silica gel chromatography (elution solvent; hexane:ethyl acetate=20:1)

출처 및 근거

ORD 기록
ord-8e51b95470514f07988902eac63c54b0
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08026370B2

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