HRID3662

反应详情

EQUATION

反应方程式

HRID 3662 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Dissolve trans-2-phenylcyclopentanecarboxylic acid (3,5-diallyl-2-amino-4,6-dioxo-cyclohex-1-enyl)amide (300 mg, 0.76 mmol) in ethanol (100 ml), add 10% potassium hydroxide (100 ml) and heat the reaction to 60° C. for 4 hours. Cool the reaction and dilute with water (200 ml). Acidify with concentrated hydrochloric acid and extract with diethyl ether (400 ml). Rinse the organic extract with water (200 ml), saturated sodium chloride (200 ml), dry over anhydrous magnesium sulfate, filter and concentrate under vacuum. Purify the residue by radial chromatography (40% to 50% ethyl acetate/hexane, 2 mm plate) to provide 5,7-diallyl-2-(2-phenylcyclopentyl)-1,7-dihydrobenzoimidazole-4,6-dione (149 mg).

WORKUP

后处理

  1. temperatureheat
  2. customthe reaction to 60° C. for 4 hours
  3. temperatureCool
  4. customthe reaction
  5. extractionAcidify with concentrated hydrochloric acid and extract with diethyl ether (400 ml)
  6. washRinse the
  7. extractionorganic extract with water (200 ml), saturated sodium chloride (200 ml)
  8. dry with materialdry over anhydrous magnesium sulfate
  9. filtrationfilter
  10. concentrationconcentrate under vacuum
  11. customPurify the residue by radial chromatography (40% to 50% ethyl acetate/hexane, 2 mm plate)