Process for producing silyl phosphine compound and silyl phosphine compound

Patent metadata

Field	Value
Publication number	US-10934316-B2
Application number	US-201716332176-A
Country	US
Kind code	B2
Filing date	Sep 19, 2017
Priority date	Sep 29, 2016
Publication date	Mar 2, 2021
Grant date	Mar 2, 2021

Abstract

The process for producing a silyl phosphine compound of the present invention comprises a first step of mixing a solvent having a relative dielectric constant of not more than 4, a basic compound, a silylating agent and phosphine to obtain a solution containing a silyl phosphine compound, a second step of removing the solvent from the solution containing a silyl phosphine compound to obtain a concentrated solution of a silyl phosphine compound, and a third step of distilling the concentrated solution of a silyl phosphine compound to obtain the silyl phosphine compound. The silyl phosphine compound of the present invention is a silyl phosphine compound represented by the following general formula (1), wherein a content of a compound represented by the following general formula (2) is not more than 0.5 mol %. (For explanatory notes of the formulas, see the specification.)

First claim

The invention claimed is:

1. A process for producing a silyl phosphine compound, comprising:
a first step of mixing a solvent, a basic compound, a silylating agent and phosphine to obtain a solution containing a silyl phosphine compound, wherein the solvent is one or two or more selected from pentane, n-hexane, n-heptane, n-octane, cyclohexane, benzene, toluene and p-xylene;
a second step of removing the solvent from the solution containing a silyl phosphine compound to obtain a concentrated solution of a silyl phosphine compound; and
a third step of distilling the concentrated solution of a silyl phosphine compound to obtain the silyl phosphine compound.

2. The process for producing a silyl phosphine compound according to claim 1 , wherein the silylating agent is a compound represented by the following general formula (I), and the silyl phosphine compound is a compound represented by the following general formula (1):

wherein each R is independently an alkyl group having not less than 1 and not more than 5 carbon atoms or an aryl group having not less than 6 and not more than 10 carbon atoms, and X is at least one group selected from a fluorosulfonic acid group, a fluoroalkanesulfonic acid group and a perchloric acid group,

wherein R is the same as in the general formula (I).

3. The process for producing a silyl phosphine compound according to claim 1 , wherein the basic compound is one or two or more selected from methylamine, diethylamine, trimethylamine, ethylamine, dimethylamine, triethylamine, ethylenediamine, aniline, toluidine, pyridine and piperidine.

4. The process for producing a silyl phosphine compound according to claim 1 , wherein the silylating agent is one or two or more selected from trimethylsilyl trifluoromethanesulfonate, triethyl silyl trifluoromethanesulfonate, tributyl silyl trifluoromethanesulfonate, triisopropyl silyl trifluoromethanesulfonate and triphenyl silyl trifluoromethanesulfonate.

5. The process for producing a silyl phosphine compound according to claim 1 , wherein the basic compound in an amount not less than 3 times and not more than 6 times the molar amount of phosphine is mixed with phosphine in the first step.

6. The process for producing a silyl phosphine compound according to claim 1 , wherein the silylating agent in an amount not less than 3 times and not more than 6 times the molar amount of phosphine is mixed with phosphine in the first step.

7. The process for producing a silyl phosphine compound according to claim 1 , wherein the silyl phosphine compound is tris(trimethylsilyl)phosphine.

8. The process for producing a silyl phosphine compound according to claim 1 , wherein the first step is carried out in an inert atmosphere.

9. The process for producing a silyl phosphine compound according to claim 1 , wherein the silyl phosphine compound obtained in the third step is mixed with an organic solvent having been dehydrated, to obtain a silyl phosphine compound in a state of being dispersed in the organic solvent.

Assignees

• Nippon Chemical Ind

Inventors

• Takubo Yosuke
• Tamura Ken

Classifications

• C07F9/06 Primary

  without P—C bonds · CPC title

• C01B25/087

  of gallium or indium · CPC title

• C07F9/062 Primary

  Organo-phosphoranes without P-C bonds · CPC title