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US 9,221,856 B2Granted
Method for purifying a crude PNPNH compound
AssigneesSaudi Basic Industries Corporation, Linde Aktiengesellschaft
InventorsUwe Rosenthal, Bernd H. Müller, Normen Peulecke, Marco Harff, Anina Wöhl, Andreas Meiswinkel, Heinz Bölt, Wolfgang Müller, Abdullah Mohammad Al-Qahtani, Mohammed H. Al-Hazmi, Shahid Majeed Azam
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Abstract
The present invention relates to a method for purifying a crude PNPNH compound by metalation and re-protonation.
Claims18
A method for purifying a crude PNPNH compound of the general structure
- R1R2P—N(R3)—P(R4)—N(R5)—H
- wherein R1, R2, R3, R4 and R5 are independently halogen, amino, trimethylsilyl, C1-C10-alkyl, substituted C1-C10-alkyl, C6-C20-aryl and substituted C6-C20-aryl, or any cyclic derivative wherein at least one of the P or N atoms of the PNPN—H structure is a member of a ring system, the ring system being formed from one or more constituent compounds of the PNPNH-structure by substitution,
- comprising:
- a) dissolving the PNPNH-compound in a first solvent;
- b) metalating the PNPNH-compound,
- c) isolating the metalated compound obtained in step b),
- d) re-protonating the metalated compound in a second solvent, and
- e) optionally removing the second solvent and optionally recrystallizing the re-protonated PNPNH ligand.
5 more elements
A method for purifying a crude PNPN—H compound comprising a PNPN—H ligand of the general structure
- R1R2P—N(R3)—P(R4)—N(R5)—H
- wherein R1, R2, R3, R4 and R5 are independently halogen, amino, trimethylsilyl, C1-C10-alkyl, substituted C1-C10-alkyl, C6-C20-aryl and substituted C6-C20-aryl, or any cyclic derivative wherein at least one of the P or N atoms of the PNPN—H structure is a member of a ring system, the ring system being formed from one or more constituent compounds of the PNPN—H-structure by substitution, and an impurity,
- the method comprising:
- (i) dissolving the crude PNPN—H compound in a first solvent;
- (ii) metalating the PNPN—H ligand,
- (iii) separating the metalated PNPN—H ligand from the first solvent and the impurity,
- (iv) re-protonating the metalated PNPN—H ligand in a second solvent, and
- (v) optionally removing the second solvent and optionally recrystallizing the re-protonated PNPNH ligand,
- to provide a purified PNPN—H compound.
6 more elements
Dependencies are inferred from the claim text.