六氯乙烷 → 4-甲氧基-3-甲基苯甲基氯

HRID 1766122

反应方程式

HRID 1766122 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 (2.31 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.

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-a1724a0eac754ee096eaff487264dfc8
来源数据集
uspto-grants-2007_06
专利号
US07229998B2

关联笔记

加载中…