Hexachloroethane → 4-Methoxy-3-methylbenzyl chloride

HRID 270155

反応式

HRID 270155 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 1437424-Methoxy-3-methylbenzyl chloride収率 100%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-b9176512d903468e9f304292a891a365
出典データセット
uspto-grants-2008_11
特許番号
US07449468B2

関連ノート

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