HRID1966961

反应详情

EQUATION

反应方程式

HRID 1966961 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

33 mg of 4-{3-[(2,6-diisopropylphenylcarbamoyl)-methyl]-2,4-dioxo-1,3-diazaspiro[4.5]dec-1-yl}benzoic acid ethyl ester are dissolved in 10 ml of methanol, 1 drop of concentrated sulfuric acid is added and the solution is refluxed for 18 hours. The mixture is stirred at reflux for 72 hours. The solvent is evaporated off. The residue is dissolved in DCM, heptane is added until slight cloudiness appears, and the solution is stirred at room temperature under nitrogen for 16 hours. The product 4-{3-[(2,6-diisopropylphenylcarbamoyl)methyl]-2,4-dioxo-1,3-diaza-spiro[4.5]dec-1-yl}benzoic acid methyl ester is obtained in the form of fine white needles.

WORKUP

后处理

  1. temperaturethe solution is refluxed for 18 hours
  2. temperatureat reflux for 72 hours
  3. customThe solvent is evaporated off
  4. dissolutionThe residue is dissolved in DCM
  5. additionheptane is added until slight cloudiness
  6. stirringthe solution is stirred at room temperature under nitrogen for 16 hours