反应 #2586801
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05468704
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a suspension of 1.6 g of NaH at 80% by weight in 42 ml of anhydrous tetrahydrofurane are added dropwise 8 g of 2,2,4,6,6-pentamethyl-3,5-heptanedione (0.04 moles). The content is stirred at ambient temperature until a homogeneous solution is obtained. 7.7 ml of methyl iodide are then added and a white precipitate forms almost immediately. The content is allowed to agitate at ambient temperature for 12 hours and then the solvent is evaporated. Some water is added (10 ml) and the content is extracted with ether and then anhydrated on Na2SO4. The ether is evaporated to the rotavapor, isolating a white needle-shaped solid, which is then purified by way of sublimation. is obtained to agitate at ambient temperature for 12 hours the solvent is evaporated Some water is added (10 ml) the content is extracted with ether The ether is evaporated to the rotavapor isolating a white needle-shaped solid, which is then purified by way of sublimation
来源 ID: ord-c5707755485c42bd9fe11d595d0c79c4