Carbon Tetrachloride → 1-(Chloromethyl)-4-propylbenzene

HRID 914479노트

반응식

HRID 914479 반응식
[CH2:1]([C:4]1[CH:9]=[CH:8][C:7]([CH2:10]O)=[CH:6][CH:5]=1)[CH2:2][CH3:3].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)(Cl)(Cl)[Cl:32]>>[Cl:32][CH2:10][C:7]1[CH:8]=[CH:9][C:4]([CH2:1][CH2:2][CH3:3])=[CH:5][CH:6]=1

참가 물질

4

반응물 3

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 2760472(4-Propylphenyl)methanol

생성물 1

HCID 122531731-(Chloromethyl)-4-propylbenzene

실험 절차

(4-Propylphenyl)methanol (4.93 g) synthesized in Reference Example 36 was dissolved in carbon tetrachloride (65 mL), triphenylphosphine (9.5 g) was added thereto, and the mixture was heated under reflux for 4 hr. The reaction mixture was concentrated under reduced pressure, and 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) to give the title compound (2.24 g) 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)

출처 및 근거

ORD 기록
ord-11ab0712b6b94be5bfe5a295786ff946
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08026370B2

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