461-18-7Relevant articles and documents
Novel synthesis method of 4, 4, 4-trifluoro-1-butanol and homologue thereof
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Paragraph 0032; 0039-0050, (2021/05/12)
The invention discloses a novel synthesis method of 4, 4, 4-trifluoro-1-butanol and a homologue thereof, and relates to the technical field of organic synthesis. The method mainly comprises the following steps of: (1) reacting ethyl trifluoroacetate with a Grignard reagent to prepare benzyloxy substituted alkyl-trifluoromethyl ketone; (2) carrying out reduction reaction on the benzyloxy substituted alkyl-trifluoromethyl ketone to prepare 1-benzyloxy-trifluorosubstituted alkyl; and (3) carrying out hydrolysis on the 1-benzyloxy-trifluorosubstituted alkyl, so as to prepare 4, 4, 4-trifluoro-1-butanol or a homologue thereof disclosed by the invention. Compared with the prior art, Freon raw materials which can pollute air are not used; dangerous lithium aluminum hydride is not used; high-temperature reaction is not needed; and the raw material ethyl trifluoroacetate is cheap and easily available, and the other main raw material Grignard reagent can also be synthesized from cheap raw materials.
Method for preparing 4,4,4-trifluoro-1-butanol
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Paragraph 0066; 0071; 0072; 0074; 0079; 0080; 0081; 0086, (2019/02/26)
The invention provides a method for preparing 4,4,4-trifluoro-1-butanol. The method comprises the following steps: A) under the action of a first catalyst, carrying out an addition reaction on 3-chloropropanol with 3,4-dihydropyran so as to prepare 2-(3-chlorine propoxy) terthydro-2H-pyran; B) under the action of a second catalyst, carrying out a cross coupling reaction on halogen fluoroform withthe 2-(3-chlorine propoxy) terthydro-2H-pyran obtained in the step A) so as to obtain 2-(4,4,4-trifluoro-butoxy) terthydro-2H-pyran; and C) under the action of a third catalyst, carrying out an elimination reaction on the 2-(4,4,4-trifluoro-butoxy) terthydro-2H-pyran obtained in the step B), thereby obtaining 4,4,4-trifluoro-1-butanol. The method is low in preparation cost, beneficial to industrialization, in addition, short in process route, high in total reaction yield, gentle in reaction condition and high in product purity.
Novel synthesis method for 4,4,4-trifluorobutanol
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Paragraph 0058; 0059; 0060; 0061; 0062; 0063, (2016/10/08)
The invention relates to a novel synthesis method for 4,4,4-trifluorobutanol. The method comprises the following steps: (1) enabling diethyl malonate to be subjected to substitution reaction with 2,2,2-trifluoro ethyl p-toluenesulfonate under the catalysis of a basic catalyst, so as to obtain 2-(2,2,2-trifluoro ethyl)-diethyl malonate; (2) enabling 2-(2,2,2-trifluoro ethyl)-diethyl malonate to be subjected to decarboxylic reaction, so as to obtain 4,4,4-trifluoro ethyl butyrate; and (3) reducing 4,4,4-trifluoro ethyl butyrate by a reduction reagent under the catalysis of a catalyst, thereby obtaining 4,4,4-trifluorobutanol. Compared with the prior art, the method disclosed by the invention has the advantages that the raw materials are cheap and readily-available, the cost is low, the number of synthesis steps is small, the operation is convenient and safe, the aftertreatment is simple, the solvent can be cyclically applied mechanically and is environment-friendly, the reaction yield is high, and the product is high in purity and good in quality and is applicable to industrial application.