With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.647-42-7, name is 3,3,4,4,5,5,6,6,7,7,8,8,8-Tridecafluorooctan-1-ol, molecular formula is C8H5F13O, molecular weight is 364.1, as common compound, the synthetic route is as follows.HPLC of Formula: C8H5F13O
Weigh 2.2 g of succinic anhydride in a 250 ml dry anhydrous three-necked flask.After filling with nitrogen for 10 min, the air in the flask and a small amount of water in the reaction system were replaced.80 ml of anhydrous ethylene glycol dimethyl ether was added to the reaction system.After pyridine 0.15ml, the temperature was raised to 75 C, 7.28 g of trifluoro-n-octanol and 40 ml of ethylene glycol dimethyl ether were gradually added dropwise to the reaction system, and the addition process was carried out to ensure that the temperature of the reaction system was controlled at 65-75 C, and the addition was completed. Rear,The reaction was maintained at 75 C for 18 h, and the reaction was stopped after 18 h.After the reaction, a certain amount of saturated NaHCO3 was added to the reaction system, and the succinic acid monoester acid was converted into a sodium salt dissolved in water. Then, a certain amount of ethyl acetate is poured into the reaction system, and unreacted fluoroalcohol, succinic anhydride and the reaction to form a succinic acid diester are dissolved in the organic phase, and the monoester acid is dissolved in the aqueous phase, and the aqueous phase is separated.The obtained aqueous phase is placed in an ice water bath, acidified with concentrated hydrochloric acid, and extracted with a certain amount of ethyl acetate, and the extract is dried with a certain amount of anhydrous magnesium sulfate.Distillation under reduced pressure gave a purer succinic acid monoester acid. The synthetic route is as follows:
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; Jiangsu Han Tuo Optical Materials Co., Ltd.; Fu Zhiwei; Song Hongbo; Dai Junyan; Ran Ruicheng; Mao Guoping; (23 pag.)CN108997182; (2018); A;,
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