HRID499753

反应详情

EQUATION

反应方程式

HRID 499753 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Tin (II) chloride (13.6 g (60 mmole)) is added to a solution of 4-(3-Nitro-phenoxymethyl)-biphenyl (4.6 g, 15 mmole) in 120 ml methanol. The reaction mixture is refluxed for 12 hr. The reaction is cooled to room temperature, 4 N of NaOH solution is added with stirring to adjust pH=8. The resulting mixture is filtered through a plug of CELITE, the filtrate concentrated and taken up in ethyl acetate. The organic layer is washed with brine and dried over Na2SO4, and concentrated. The resulting solid is washed with little methanol to yield 3-(Biphenyl-4-ylmethoxy)-aniline as a yellow solid. MS: 276(M+1).

WORKUP

后处理

  1. temperatureThe reaction mixture is refluxed for 12 hr
  2. filtrationThe resulting mixture is filtered through a plug of CELITE
  3. concentrationthe filtrate concentrated
  4. washThe organic layer is washed with brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated
  7. washThe resulting solid is washed with little methanol