反应 #3474483
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06906103B2
反应条件: temp:97.51; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Pyrrole-2,5-dicarbaldehyde (0.21 g, 1.71 mmol) was dissolved in 35 ml of hot water and placed in a hot water bath (95-100° C.). A solution of KMnO4 (0.788 g, 5.13 mmol) in 10 ml of water was added dropwise in a period of 5 min. The reaction mixture was stirred at 95-100° C. for 1 h, and was then cooled to 70° C. The brown precipitates (MnO2) were filtered off and washed with water. The filtrate was acidified at 0° C. with 5 M HCl to pH 2, evaporated to dryness, and dried under high vacuum. The product was dissolved in 80 ml of anhydrous EtOH and the solution was filtered through a funnel. The filtrate was evaporated to give a brown solid (0.25 g), which was used in next reaction without further purification. ESI MS: 154.00 (M−H+). 1H NMR (DMSO-d6) δ 12.68 (br. S), 12.17 (s), 6.72 (s). placed in a hot water bath (95-100° C.) was then cooled to 70° C The brown precipitates (MnO2) were filtered off washed with water was acidified at 0° C. with 5 M HCl to pH 2 evaporated to dryness dried under high vacuum The product was dissolved in 80 ml of anhydrous EtOH the solution was filtered through a funnel The filtrate was evaporated
来源 ID: ord-f9bf39dbfe134a8dab74655df013ed93