Abstract

The present invention relates to the field of organic chemistry, and in particular relates to a preparation method for lithium bisfluorosulfonylimide. The preparation method comprises: reacting bisfluorosulfonylimide with lithium carbonate in a mixed organic solvent, and performing a post-treatment to obtain lithium bisfluorosulfonylimide. In the synthesis route of the present application, the reaction process stays at the stage of lithium bicarbonate, such that the reaction system contains very little water, and the resulting lithium bicarbonate is extremely easily recovered. Moreover, the process method of the present application is simple, and lithium bisfluorosulfonylimide with a high yield and a high quality can be prepared.

IPC Classes  ?

• C01B 21/086 - Compounds containing nitrogen and non-metals containing one or more sulfur atoms

Abstract

A first aspect of the present invention provides a method for the preparation of 2-chloro-5-chloromethylpyridine, comprising: performing a cyclization reaction on 4,5-dichloro-4-methoxypentanenitrile in presence of a silicon compound and an acylamide compound to obtain 2-chloro-5-chloromethylpyridine. Another aspect of the present invention provides a method for preparation of 2-(chloromethyl)-5-(trifluoromethyl)-1,3,4-oxadiazole, comprising: performing a cyclization reaction on 1-(chloroacetyl)-2-(trifluoroacetyl)hydrazine in a presence of a silicon compound and an acylamide compound to obtain 2-(chloromethyl)-5-(trifluoromethyl)-1,3,4-oxadiazole. The silicon compound or/and acylamide compound provided by the present invention serve as cyclization reagents and have high efficiency.

IPC Classes  ?

• C07D 213/61 - Halogen atoms or nitro radicals
• B01J 31/02 - Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
• C07D 271/10 - 1,3,4-OxadiazolesHydrogenated 1,3,4-oxadiazoles

Abstract

The present invention relates to the field of organic chemistry, and in particular, relates to a use of a silicon compound in a cyclization reaction. On one hand, the present invention provides a method for preparing 2-chloro-5-chloromethylpyridine, comprising: performing a cyclization reaction on 4-aldehydo-4,5-dichlorovaleronitrile in the presence of a silicon compound and an amide compound, so as to provide the 2-chloro-5-chloromethylpyridine. On the other hand, the present invention provides a method for preparing 5-chloromethyl-2-trifluoromethyl-1,3,4-oxadiazole, comprising: performing a cyclization reaction on 1-(chloroacetyl)-2-(trifluoroacetyl)hydrazine in the presence of a silicon compound and an amide compound, so as to provide the 5-chloromethyl-2-trifluoromethyl-1,3,4-oxadiazole. By using the silicon compound or/and amide provided by the present invention as a cyclization reagent, cyclization synthesis can be efficiently performed.

IPC Classes  ?

• C07D 213/61 - Halogen atoms or nitro radicals
• C07D 271/10 - 1,3,4-OxadiazolesHydrogenated 1,3,4-oxadiazoles

Abstract

Provided is a preparation method for lithium bis-(fluoro-sulfonyl) imide, comprising the following steps: (1) carrying out fluorination: synthesizing an intermediate bis-(fluoro-sulfonyl) imide by using bis-(chloro-sulfonyl) imide and hydrogen fluoride in presence of a catalyst; and (2) enabling the obtained bis-(fluoro-sulfonyl) imide and alkaline lithium to react, and carrying out solid-liquid separation after the reaction to obtain the lithium bis-(fluoro-sulfonyl) imide. The preparation method is low in cost, fewer in by-products and simple in aftertreatment, and is capable of guaranteeing the quality and purity of products, thereby being suitable for industrial production.

IPC Classes  ?

• C01B 21/096 - Amidosulfonic acidSalts thereof