# US 2016/0251384 A1 · Method of separating acids from chemical reaction mixtures by means of apolar amines

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- Number: US 2016/0251384 A1
- Document ID: US20160251384A1
- Status: Published application
- Kind: A1
- Application number: 15/148,430
- Filed: 2016-05-06
- Published: 2016-09-01
- Earliest claimed: 2005-11-08
- Assignees: BASF SE
- Applicants: BASF SE
- Inventors: OLIVER HUTTENLOCH; Patrick DECK; Holger GANZ; Michael MAUSS; Wolfgang KÖRNIG; Martin BOCK
- Web page: https://patentgrep.com/patent/US20160251384A1

## CPC

- C07F 9/224: {Phosphorus triamides}
- C07B 63/00: Purification; Separation (separation of optically-active compounds C07B57/00); Stabilisation; Use of additives
- C07F: ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM (metal-containing porphyrins C07D487/22)
- C07B: GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR (preparation of carboxylic acid esters by telomerisation C07C67/47; telomerisation C08F)

## Abstract

A process for the removal of acids from reaction mixtures, comprising at least one product of value which is sparingly soluble in water, by at least one unpolar amine as an auxiliary base, which includes: a) reacting the auxiliary base with the acid with formation of a salt; b) reacting the salt formed in step a) with a further base which accepts the acid with liberation of the auxiliary base and combines with the acid to be accepted from the auxiliary base to form a salt which is very readily soluble in water; c) extraction of the mixture obtained in step b) with water or an aqueous medium, wherein the salt of the further base dissolves in the aqueous phase and the product of value, or the solution of the product of value, in a suitable solvent and the auxiliary base form at least one separate nonaqueous phase; and d) removal by distillation of at least part of any solvent present from the at least one nonaqueous phase obtained in step c), to form two nonmiscible liquid phases.

## Claims

### Claim 1

(canceled)

### Claim 2 (depends on 7)

The process according to claim 7, wherein the auxiliary base is separated off and recirculated into the process.

### Claim at position 3

3-6. (canceled)

### Claim 7

A process for the preparation of thiophosphoric triamides by reacting thiophosphoryl chloride with at least one primary or secondary amine in an inert solvent with the aid of at least one unpolar amine as an auxiliary base, comprising the following steps:
a) reacting the auxiliary base with the hydrogen chloride formed during the reaction, with formation of a chloride salt;
b) reacting the chloride salt formed in step a) with ammonia, which accepts the hydrogen chloride with liberation of the auxiliary base;
c) extracting the mixture obtained in step b) with water or an aqueous medium, wherein ammonium chloride formed dissolves in the aqueous phase and the solution of the product of value in the inert solvent and the auxiliary base form at least one separate nonaqueous phase; and
d) removing by distillation of at least some of the inert solvent from the at least one nonaqueous phase obtained in step c), to form two nonmiscible liquid phases.

### Claim 8

(canceled)

### Claim 9 (depends on 7)

The process according to claim 7, wherein the auxiliary base is a tertiary amine.

### Claim at position 7

10-11. (canceled)

### Claim 12 (depends on 7)

The process according to claim 7, wherein the auxiliary base is triethylamine, tri-n-propylamine or tri-n-butylamine.

### Claim at position 9

13-16. (canceled)

### Claim 16 (depends on 7)

The process according to claim 7, wherein the acid is liberated during the course of a phosphorylation or thiophosphorylation reaction.

### Claim at position 11

17-20. (canceled)