Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 647-42-7, name is 3,3,4,4,5,5,6,6,7,7,8,8,8-Tridecafluorooctan-1-ol. A new synthetic method of this compound is introduced below., 647-42-7
The corresponding fluoroalcoholic substrate 1e (0.728 g, 2.0 mmol) was added to the reaction flask and anhydrous DMF (3 mL) was added.Additional DSC (0.613 g, 1.2 eq.) and pyridine (0.16 mL, 1.0 eq.).The mixture was heated at 40 C for 15 h.It was monitored by TLC until the alcohol was completely reacted. Cool the mixture to room temperature,Boc-t-Bu-lysine (0.604 g, 2.0 mmol) was added.Keep the temperature below 30 C.The reaction mixture was then stirred at room temperature overnight.It was monitored by TLC until the starting material was complete.Water (10 mL) and ethyl acetate (10 mL) were added to the mixture.The organic layer was separated and the aqueous layer was evaporated elutCombine the two organic layers, using 1 mol/L hydrochloric acid in sequence.Wash with water and saturated brine,It was dried over anhydrous magnesium sulfate. Concentrate the organic solution,Fluorine-containing amino acid derivative precursor obtained by flash column chromatography3e (0.598g, 1.86mmol),The yield is 93%.Purity is 99%,It is an oily substance.
At the same time, in my other blogs, there are other synthetic methods of this type of compound,647-42-7, 3,3,4,4,5,5,6,6,7,7,8,8,8-Tridecafluorooctan-1-ol, and friends who are interested can also refer to it.
Reference:
Patent; Shanghai Institute of Technology; Liu Meina; Zhu Yu; Wu Tong; Deng Wei; Xuan Maojie; Miao Dengyun; Liu Zhifeng; Shan Yu; (13 pag.)CN108997168; (2018); A;,
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