Hexachloroethane → 4-Methoxy-3-methylbenzyl chloride

HRID 270155

반응식

HRID 270155 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9]O)=[CH:5][C:4]=1[CH3:11].[Cl:12]C(Cl)(Cl)C(Cl)(Cl)Cl.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C(Cl)Cl>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][Cl:12])=[CH:5][C:4]=1[CH3:11]

참가 물질

5

반응물 3

HCID 6214HexachloroethaneHCID 11776TriphenylphosphineHCID 14457544(4-Methoxy-3-methylphenyl)methanol

생성물 1

HCID 1437424-Methoxy-3-methylbenzyl chloride수율 100%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a stirred solution of (4-methoxy-3-methylphenyl)methanol (2.31g, 15.18mmoles, 1eq) in anhydrous CH2Cl2(50ml, 0.3M) was added hexachloroethane (3.59g, 15.18mmoles, 1eq) and triphenylphosphine (3.98g, 15.18mmoles, 1eq). This mixture was stirred at room temperature overnight at which point the reaction was transferred to a separatory funnel and washed with H2O, brine, dried over Na2SO4, filtered, concentrated in vacuo and filtered through a plug of silica gel (30% EtOAc/Hexanes) to yield 2.59g (100%) of product.

후처리

  1. customwas transferred to a separatory funnel
  2. washwashed with H2O, brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. filtrationfiltered through a plug of silica gel (30% EtOAc/Hexanes)

출처 및 근거

ORD 기록
ord-b9176512d903468e9f304292a891a365
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07449468B2

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