反应 #1295750
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09085586B2
反应条件: temp:180.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A solution of 1,3-diethyl 2-(3-oxocyclohexyl)propanedioate (28.50 g, 111.20 mmol, 1.00 equiv) and sodium chloride (7.02 g, 1.10 equiv) in a mixture of water (4 mL)/DMSO (80 mL) was heated for 24 h at 180° C. in an oil bath. After cooled down to r.t, the reaction was then diluted with water, extracted with 3×300 mL of ethyl acetate. The organic layers were combined, washed with water and brine, dried over anhydrous sodium sulfate and concentrated under vacuum to give ethyl 2-(3-oxocyclohexyl)acetate (22.7 g, crude) as yellow oil which was used for next step without purification. After cooled down extracted with 3×300 mL of ethyl acetate washed with water and brine dried over anhydrous sodium sulfate concentrated under vacuum
来源 ID: ord-3fcd02889b0048589ba3d482638b605e