Hexachloroethane → 4-Methoxy-3-methylbenzyl chloride

HRID 1766122

반응식

HRID 1766122 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 (2.31 g, 15.18 mmoles, 1 eq) in anhydrous CH2Cl2 (50 ml, 0.3M) was added hexachloroethane (3.59 g, 15.18 mmoles, 1 eq) and triphenylphosphine (3.98 g, 15.18 mmoles, 1 eq). 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 2.59 g (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-a1724a0eac754ee096eaff487264dfc8
출처 데이터셋
uspto-grants-2007_06
특허 번호
US07229998B2

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