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Method for preparing bis(diphenylphosphino)

A bis-diphenylphosphine-alkane and diphenylphosphine-alkane technology, which is applied in the field of synthesis of bidentate phosphine ligands, can solve the problems of difficult large-scale industrial application, complicated operation, complicated equipment, etc., and achieves convenient and simplified operation The effect of small investment in steps and equipment

Inactive Publication Date: 2015-04-29
HENAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Ma Huailing and others used ultrasonic-assisted reaction to synthesize such ligands with a yield of more than 90%. However, this method needs to remove unreacted metal lithium and by-product phenyllithium, etc., and the operation is complicated. At the same time, ultrasonic reaction is currently in the laboratory stage. Even if it can be industrialized in the future, there are disadvantages such as large investment and complicated equipment, so this method is difficult to apply in large-scale industrialization

Method used

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  • Method for preparing bis(diphenylphosphino)

Examples

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Effect test

Embodiment 1

[0015] Synthesis of Bis-diphenylphosphineethane

[0016] Add 600L tetrahydrofuran and 15kg lithium metal to a 1000L reactor, add 220kg diphenylphosphine chloride dropwise at 20°C, after the reaction of diphenylphosphine chloride is complete, add 49kg 1,2-dichloroethane dropwise at 20°C After the reaction is completed, add 1kg antioxidant 300, remove THF under reduced pressure, add 400L 2M dilute hydrochloric acid, stir, cool, and centrifugally filter. The filter cake is recrystallized with 300L methanol to obtain 189kg white solid bis-diphenylphosphineethane with a purity of 96 %, yield 95%.

Embodiment 2

[0018] Synthesis of bis-diphenylphosphinopropane

[0019] Add 650L tetrahydrofuran and 16kg lithium metal to a 1000L reactor, add 220kg diphenylphosphine chloride dropwise at 60°C, after the reaction of diphenylphosphine chloride is complete, add 56.5kg 1,3-dichloropropane dropwise at 60°C After the reaction was completed, 1.5kg of antioxidant 300 was added, THF was removed under reduced pressure, 450L of 2M dilute hydrochloric acid was added, stirred, cooled, centrifugally filtered, and the filter cake was recrystallized with 350L of methanol to obtain 198kg of white solid bis-diphenylphosphinopropane with a purity of 96 %, yield 96%.

Embodiment 3

[0021] Synthesis of bis-diphenylphosphinobutane

[0022] Add 700L tetrahydrofuran and 15kg lithium metal to a 1000L reactor, add 220kg diphenylphosphine chloride dropwise at 40°C, after the reaction of diphenylphosphine chloride is complete, add 62.5kg 1,4-dichlorobutane dropwise at 50°C Alkanes, after the reaction is completed, add 2kg antioxidant 264, remove tetrahydrofuran under reduced pressure, add 500L 2M dilute hydrochloric acid, stir, cool, and centrifugally filter, and the filter cake is recrystallized with 400L methanol to obtain 207kg white solid bis-diphenylphosphinobutane. 96%, yield 97%.

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Abstract

The invention discloses a method for preparing bis(diphenylphosphino), and belongs to the technical field of diphosphine ligands. According to the technical scheme, the method for preparing bis(diphenylphosphino) comprises the following steps: adding tetrahydrofuran and a lithium metal into a reaction kettle, dropwise adding chlorodiphenylphosphine at 20-60 DEG C, dropwise adding dichloralkane at 20-60 DEG C after the chlorodiphenylphosphine is completely reacted, adding an amino antioxidant or a phenol antioxidant after the reaction is completed, depressurizing, removing tetrahydrofuran, adding diluted hydrochloric acid, filtering, and recrystallizing the filter cakes, thereby obtaining bis(diphenylphosphino). The method disclosed by the invention is typical one-pot reaction, is small in equipment investment, simple in equipment and convenient to operate, and due to addition of the antioxidant, the operation steps are greatly simplified, and the yield of the product is increased.

Description

technical field [0001] The invention belongs to the technical field of synthesis of bidentate phosphine ligands, and in particular relates to a preparation method of bis-diphenylphosphine alkane. Background technique [0002] Organophosphine ligands are one of the most widely used and most functional ligands in contemporary homogeneous catalysis, and are widely used in many fields such as basic theoretical research and large-scale industrial production. Compared with other ligands, organic phosphine ligands have superior electronic effects and steric effects, and can form complexes with novel spatial structures and excellent catalytic properties with many metal salts. Therefore, the synthesis and properties of such ligands It has always been a research hotspot. In recent years, with the deepening of theoretical research on homogeneous catalysis, the research on bidentate phosphine ligands has attracted more and more attention. The research results on the modification of or...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/50
Inventor 轩小朋梁蕊李玉江赵培正崔延瑞
Owner HENAN NORMAL UNIV
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