HRID1701972

反应详情

EQUATION

反应方程式

HRID 1701972 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1.6 g of N-(4-[2-amino-ethyl]-benzenesulfonyl)-N'-cyclohexyl urea and 0.2 g of sodium hydroxide are dissolved in 10 ml of water and 50 ml of acetone. With agitation and ice cooling, a solution of 0.85 g of 4-methyl-2-oxo-piperidine-1-carboxylic acid chloride (prepared by reaction of the sodium compound of 4-methyl-2-oxo-piperidine with phosgene) in 20 ml of acetone is added dropwise to this solution, and agitation is continued for 2 hours at room temperature. Subsequently, the acetone is evaporated under reduced pressure, the batch is acidified, suction-filtered, the product is reprecipitated from dilute ammonia and recrystallized from dilute acetone. The N-(4-[2-(4-methyl-2-oxo-piperidine-1-carboxamido)-ethyl]-benzenesulfonyl)-N'-cyclohexyl urea obtained has a melting point of 177°-178° C. and is identical with the product obtained according to Example 8.

WORKUP

后处理

  1. additionis added dropwise to this solution, and agitation
  2. customSubsequently, the acetone is evaporated under reduced pressure
  3. filtrationsuction-filtered
  4. customthe product is reprecipitated from dilute ammonia
  5. customrecrystallized from dilute acetone