反应 #3755016
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08088955B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A solution of 2-(3-(methoxypropoxy)-4-methoxybenzylidene) -3-methylbutanal (7.0 mmol, 74% E and 26% Z), tetrarhodium dodecacabonyl (0.14 mmol), (2R,3R)-(+)-2,3-Bis-(Diphenylphosphino)butane (R, R-Chiraphos, 0.63 mmol) and 300 ul triethylamine in toluene (75 ml) was transferred into an autoclave. The mixture was hydrogenated at 70-80° C. and 20 bar H2. After 42 hr additional tetrarhodium dodecacarbonyl (0.14 mmol) was added to complete the reaction in 62 hr. The mixture was concentrated to 3.5 g black oil and purified by flash chromatography (heptane/ethyl acetate=2/1). Yield=1.6 g yellow oil (74%). was hydrogenated at 70-80° C. the reaction in 62 hr The mixture was concentrated to 3.5 g black oil purified by flash chromatography (heptane/ethyl acetate=2/1)
来源 ID: ord-8518ceaeebf644c89ccad75cf15a3f7f