HRID1977458

反应详情

EQUATION

反应方程式

HRID 1977458 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 4-(2-aminoethyl)aniline hydrochloride salt (10.0 g, 78 mmol) was dissolved in dioxane (200 mL) followed by the addition of 5 M HCl (14.6 ml) and water (25 ml). The solution was cooled in an ice bath and was treated quickly with benzenesulfonyl chloride (10.3 ml, 81 mmol). Pyridine (10 ml) was added and the solution stirred at ambient temperature for 16 h. The solvent was removed under reduced pressure and the residue was dissolved in water (300 ml) and washed with 3 portions of diethylether. The aqueous solution was treated with 80 ml of 5 N sodium hydroxide and was washed again with 3 portions of diethylether. The aqueous phase was adjusted to a pH of approximately 9 by the addition of 40 ml of 5N HCl. The solids were collected and dried. NMR, MS, EA.

WORKUP

后处理

  1. temperatureThe solution was cooled in an ice bath
  2. customThe solvent was removed under reduced pressure
  3. dissolutionthe residue was dissolved in water (300 ml)
  4. washwashed with 3 portions of diethylether
  5. additionThe aqueous solution was treated with 80 ml of 5 N sodium hydroxide
  6. washwas washed again with 3 portions of diethylether
  7. additionThe aqueous phase was adjusted to a pH of approximately 9 by the addition of 40 ml of 5N HCl
  8. customThe solids were collected
  9. customdried