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ChemicalBook CAS DataBase List 1-PENTANOL, 3-METHYL-5-PHENYL

1-PENTANOL, 3-METHYL-5-PHENYL synthesis

7synthesis methods
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Yield:55066-48-3 94.2%

Reaction Conditions:

with 3% Pd/silica;hydrogen;propionic acid in water at 105 - 110; under 9000.9 Torr;Autoclave;Inert atmosphere;Reagent/catalyst;Pressure;Temperature;

Steps:

9 Hydrogenation reaction to prepare 3-methyl-5-phenyl-pentanol
FeedingA mixture of 200 g of phenyl-dihydropyran,100 g of 1% propionic acid aqueous solution and 3% Pd / silica catalyst (2.5 g) were successively added to 1 L of an autoclave. The autoclave was sealed, replaced with nitrogen, and replaced with hydrogen.HydrogenationThe autoclave was heated to 105-110 ° C and the hydrogenation pressure was 1.2 MPa to start hydrogenation.Cooling, decompression, nitrogen purgeWhen the gas phase detection of raw materials remained less than 5%, the hydrogenated material down to room temperature, the hydrogen released to 0.04 ~ 0.06Mpa,Through the nitrogen to the dad pressure is not less than 0. 3Mpa, vent to 0.04 ~ 0.06Mpa, repeat the operation 3 times, and then filter, washed,The crude phase was obtained by distillation under reduced pressure. The oil phase was purified by distillation to give 3-methyl-5-phenyl-pentanol with a purity of more than 98.5%Time 7 h, selectivity 95.6%, yield 94.2%.

References:

Shandong NHU Pharmaceutical Co. Ltd;Fang, Wanjun;Ma, Xiao;Xu, Peng;Wang, Jun;Liu, Xiujuan;Li, CongCong;Guan, YaJun;Li, YuXiang;Song, Jiang CN105924332, 2016, A Location in patent:Paragraph 0029; 0030; 0031

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