HRID2104353

反应详情

EQUATION

反应方程式

HRID 2104353 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

(±)-trans-1,2-Cyclopentanediamine (WO98/30574) (692 mg) was dissolved in methylene chloride (10 mL), and to the solution were added triethylamine (1.1 mL) and 2-(tert-butoxycarbonyloxyimino)-2-phenylacetonitrile (493 mg) at 0° C., followed by stirring at 0° C. for 1 hour. Subsequently, additional 2-(tert-butoxycarbonyloxyimino)-2-phenylacetonitrile (493 mg) was added thereto, and the thus-obtained mixture was stirred at room temperature for 7 hours. Water was added to the reaction mixture to partition the mixture. The organic layer was washed with saturated brine, and was dried over sodium sulfate anhydrate. The residue was purified by silica gel flash column chromatography (methylene chloride:methanol=9:1), to thereby give the title compound (395 mg).

WORKUP

后处理

  1. stirringthe thus-obtained mixture was stirred at room temperature for 7 hours
  2. customto partition the mixture
  3. washThe organic layer was washed with saturated brine
  4. dry with materialwas dried over sodium sulfate anhydrate
  5. customThe residue was purified by silica gel flash column chromatography (methylene chloride:methanol=9:1)