HRID1602486

反应详情

EQUATION

反应方程式

HRID 1602486 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-[3-(4-Chlorophenylsulfonyl)propyl]-2-nitrophenol (10.00 g, 28.11 mmol) was dissolved in 1,4-dioxane (100 ml), 4 N hydrochloric acid solution in 1,4-dioxane (8.43 ml, 33.73 mmol) and 10% palladium-carbon (1.0 g) were added, and the mixture was stirred for 4 hours in an atmosphere of hydrogen gas under 1 atmospheric pressure. The crystals precipitated in the reaction solution were dissolved by adding methanol, the reaction mixture was filtered, and then the resulting filtrate was concentrated under reduced pressure. By crystallizing the resulting residue from acetonitrile-ether, 2-amino-4-[3-(4-chlorophenylsulfonyl)propyl]phenol hydrochloride (9.71 g, 95%) was obtained.

WORKUP

后处理

  1. customThe crystals precipitated in the reaction solution
  2. dissolutionwere dissolved
  3. additionby adding methanol
  4. filtrationthe reaction mixture was filtered
  5. concentrationthe resulting filtrate was concentrated under reduced pressure
  6. customBy crystallizing the resulting residue from acetonitrile-ether