反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureheat
- customthe reaction to 60° C. for 4 hours
- temperatureCool
- customthe reaction
- extractionAcidify with concentrated hydrochloric acid and extract with diethyl ether (400 ml)
- washRinse the
- extractionorganic extract with water (200 ml), saturated sodium chloride (200 ml)
- dry with materialdry over anhydrous magnesium sulfate
- filtrationfilter
- concentrationconcentrate under vacuum
- customPurify the residue by radial chromatography (40% to 50% ethyl acetate/hexane, 2 mm plate)