Method for purifying a crude PNPNH compound
View Patent ↗A method for purifying a crude PNPNH compound of the general structure R 1 R 2 P—N(R 3 )—P(R 4 )—N(R 5 )—H wherein R 1 , R 2 , R 3 , R 4 and R 5 are independently halogen, amino, trimethylsilyl, C 1 -C 10 -alkyl, substituted C 1 -C 10 -alkyl, C 6 -C 20 -aryl and substituted C 6 -C 20 -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, the method comprising the steps: A. a) dissolving the crude PNPNH-compound in a C 1 -C 10 alcohol or mixture thereof under heating; b) cooling the solution obtained in step a), c) precipitating the PNPNH compound, separating and optionally drying, or B. (i) washing the crude PNPNH compound with C 1 -C 10 alcohol or a mixture thereof, (ii) separating the PNPNH compound and optionally drying thereof.
1. A method for purifying a crude PNPNH compound comprising a ligand of the general structure
R 1 R 2 P—N(R 3 )—P(R 4 )—N(R 5 )—H
wherein R 1 , R 2 , R 3 , R 4 and R 5 are independently halogen, amino, trimethylsilyl, C 1 -C 10 -alkyl, substituted C 1 -C 10 -alkyl, C 6 -C 20 -aryl and substituted C 6 -C 20 -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, wherein the substitution is by formally eliminating per constituent compound either two whole groups R 1 -R 5 or H, one atom from each of two groups R 1 -R 5 or a whole group R 1 -R 5 or H and an atom from another group R 1 -R 5 , and joining the formally so created valence-unsaturated sites by one covalent bond per constituent compound to provide the same valence as initially present at a given site,
the method comprising:
A.
a) dissolving the crude PNPNH-compound in a C 1 -C 10 alcohol or mixture thereof under heating, wherein an alcohol/ligand weight ratio is from 1.0-0.3;
b) cooling the solution obtained in step a); and
c) isolating the PNPNH compound; or
B.
(i) washing the crude PNPNH compound with C 1 -C 10 alcohol or a mixture thereof;
(ii) separating the PNPNH compound; and optionally drying thereof.
2. The method according to claim 1 , wherein the crude PNPNH compound is dissolved in step a) in or is washed in step (i) with a C 1 -C 5 alcohol.
3. The method according to claim 1 , wherein man alcohol/ligand weight ratio in step B. (i) is from 5.0-0.1.
4. The method according to claim 1 , wherein the heating in step A. a) is to a temperature of about 50-100° C.
5. The method according to claim 1 , wherein the solution in step A. b) is cooled to temperature between −20 to +20° C.
6. The method according to claim 1 , wherein PNPNH seed crystals are added before or during step A. b) and/or A. c).
7. The method according to claim 1 , wherein a precipitate obtained in step A. c) is washed with C 1 -C 5 alcohol, and is then dried at 10-50° C., in a vacuum of 5.0-500 millibar.
8. The method according to claim 1 , wherein the washing in step B. (i) is at a temperature of about 0-25° C.
9. The method according to claim 1 , wherein the C 1 -C 10 alcohol is removed in step B. (ii) by drying at 10-50° C., in a vacuum of 5.0-500 millibar.
10. The method according to claim 1 , wherein the crude PNPNH compound comprises an impurity comprising ligand synthesis products, ligand reaction products with oxygen and/or water, or a combination thereof.