1,1-Diphenyl-3,3-dimethyl-1-butene synthesis
- Product Name:1,1-Diphenyl-3,3-dimethyl-1-butene
- CAS Number:23586-64-3
- Molecular formula:C18H20
- Molecular Weight:236.35
Yield:23586-64-3 78%
Reaction Conditions:
with lithium hemisulfide in N,N-dimethyl acetamide at 20; for 12 h;Schlenk technique;Inert atmosphere;Irradiation;
Steps:
32
General procedure: A redox alkyl active carboxylate (0.4 mmol) and lithium sulfide (0.04 mmol) were added to a 10 mL Schlenk reaction tube (Beijing Xinweier Glass Instrument Co., Ltd., F891410 reaction tube, capacity 10 mL, grinding mouth 14/20). The air in the tube was completely replaced three times with argon, and then 2 mL of N,N-dimethylacetamide (DMA) and a radical acceptor (0.2 mmol) were added under an argon atmosphere. The reaction system was continuously stirred at room temperature for 12 hours under the irradiation of a 40W purple LED (427 nm) lamp (IKA magnetic stirrer, RCT basic type, stirring speed 500 rpm). After the completion of the reaction, the reaction was quenched with saturated NaCl solution, and the reaction solution was repeatedly extracted 3 times with 10 mL of ethyl acetate, and the combined organic phase was concentrated by rotary evaporation (Swiss Buchi Co., Ltd., BUCHI rotary evaporator R-3 ). The concentrated residue was chromatographed on a column (Beijing Xinweier Glass Instrument Co., Ltd., C383040C spherical column with sand plate storage, 35/20, effective length: 500ml) to obtain the product. (the product is a colorless viscous liquid, eluent ethyl acetate: petroleum ether=1:50),
References:
CN114085187,2022,A Location in patent:Paragraph 0289-0295; 0358-0359; 0311-0316; 0317-0323; ...
38442-51-2
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