HRID1894858

反应详情

EQUATION

反应方程式

HRID 1894858 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

75 mg (0.54 mmol) of potassium carbonate are added to a solution of 130 mg (0.49 mmol) of 1-phenyl-2-thia-1,3-diazaspiro[4.5]decane-2,2-dioxide and 136 mg (0.54 mmol) of 2-chloro-N-(2,6-diisopropylphenyl)-acetamide in 30 ml of dimethylformamide. The reaction medium is stirred at room temperature for one night and then it is heated to reflux for 6 hours and at room temperature for 48 h. The medium is then poured into water and extracted with ethyl acetate. The organic phases are collected and washed with water. They are dried over sodium sulfate. The solvents are evaporated. The residue is chromatographed on silica gel (heptane/ethyl acetate 90/10). 125 mg of N-(2,6-diisopropylphenyl)-2-(2,2-dioxo-1-phenyl-2-thia-1,3-diazaspiro[4.5]dec-3-yl]acetamide are obtained in the form of a yellow oil. The product is triturated in dichloromethane and plenty of heptane. A solid is obtained. M.p. 140-2° C., yield=53%.

WORKUP

后处理

  1. temperatureit is heated
  2. temperatureto reflux for 6 hours and at room temperature for 48 h
  3. extractionextracted with ethyl acetate
  4. customThe organic phases are collected
  5. washwashed with water
  6. dry with materialThey are dried over sodium sulfate
  7. customThe solvents are evaporated
  8. customThe residue is chromatographed on silica gel (heptane/ethyl acetate 90/10)