六氯乙烷 → 4-甲氧基-3-甲基苯甲基氯

HRID 270155

反应方程式

HRID 270155 反应方程式
[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]

参与物

5

反应物 3

HCID 6214六氯乙烷HCID 11776三苯基膦HCID 144575444-甲氧基-3-甲基苄醇

产物 1

HCID 1437424-甲氧基-3-甲基苯甲基氯收率 100%

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂

实验过程

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.

后处理

  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)

来源与证据

ORD记录
ord-b9176512d903468e9f304292a891a365
来源数据集
uspto-grants-2008_11
专利号
US07449468B2

关联笔记

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