Method of separating acids from chemical reaction mixtures by means of apolar amines

Patent metadata

Field	Value
Publication number	US-9493491-B2
Application number	US-201615148430-A
Country	US
Kind code	B2
Filing date	May 6, 2016
Priority date	Nov 8, 2005
Publication date	Nov 15, 2016
Grant date	Nov 15, 2016

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.

First claim

We claim:

1. 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.

2. The process according to claim 1 , wherein the auxiliary base is a tertiary amine.

3. The process according to claim 1 , wherein the auxiliary base is triethylamine, tri-n-propylamine or tri-n-butylamine.

4. The process according to claim 1 , wherein the acid is liberated during the course of a phosphorylation or thiophosphorylation reaction.

5. The process according to claim 1 , wherein the auxiliary base is separated off and recirculated into the process.

Assignees

• Basf Se

Inventors

• Huttenloch Oliver
• Deck Patrick
• Ganz Holger
• Mauss Michael
• Körnig Wolfgang
• Bock Michael

Classifications

• C07B63/00

  Purification; Separation (separation of optically-active compounds C07B57/00); Stabilisation; Use of additives · CPC title

• C07F9/224 Primary

  Phosphorus triamides · CPC title