HRID461424

反应详情

EQUATION

反应方程式

HRID 461424 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

n-Propylamine (5.9 g., 0.1 mole.) and propylene carbonate (10.2 g., 0.1 mole.) were mixed and heated at 60° over night. To the resulting hydroxypropyl-n-propylcarbomate were added p-chlorobenzene sulfonamide (10.67 g., as sodium salt) and DMF (200 ml.) and the mixture was heated at 120° for 4 hours. After evaporation of the solvent the residue was taken up in water (200 ml.) and the solution adjusted to pH 8 by the addition of acetic acid. Unreacted p-chlorobenzene sulfonamide (2 g.) separated out and was collected. Further adjustment to pH 5 precipitated 1-(4-chloro-benzenesulfonyl)-3-n-propyl-urea (2 g.) whose infrared spectrum was identical with that of an authentic sample.

WORKUP

后处理

  1. temperatureheated at 60° over night
  2. temperaturethe mixture was heated at 120° for 4 hours
  3. customAfter evaporation of the solvent the residue
  4. additionthe solution adjusted to pH 8 by the addition of acetic acid
  5. customUnreacted p-chlorobenzene sulfonamide (2 g.) separated out
  6. customwas collected
  7. customFurther adjustment to pH 5 precipitated 1-(4-chloro-benzenesulfonyl)-3-n-propyl-urea (2 g.) whose