US4113783A
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Reduction of triphenylphosphine oxide to triphenylphosphine
Assignee: Texas Alkyls Inc
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Filing: 1977-06-09
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Granted: 1978-09-12
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Expires: 1997-06-09
Abstract
Abstract Triphenylphosphine oxide is reduced to triphenylphosphine by the steps of (a) reacting triphenylphosphine oxide with a dialkylaluminum hydride either formed externally to the reaction system or generated in situ by the application of heat to a trialkylaluminum in which at least one alkyl group contains from 2 to 15 carbon atoms and in which the β-carbon on said alkyl group is directly bonded to at least one hydrogen atom, and (b) hydrolyzing the product of step (a) to produce triphenylphosphine.
Inventors
- 👤 Dennis B. Malpass
- 👤 G. Scott Yeargin
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-06 16:12
CPC Classifications
C; C07; C07F; C07F9/00; C07F9/02; C07F9/28; C07F9/50; C07F9/505; C07F9/509
Claims Analysis
Total Claims: 18
Claim 1
Independent Claim
55 words
A process for the conversion of triphenylphosphine oxide to triphenylphosphine comprising the steps of (a) reacting triphenylphosphine oxide with a dialkylaluminum hydride of which the alkyl groups are the same or different and each contain from 1 to 15 carbon atoms in a straight or branched chain; and (b) hydrolyzing the product of step (a).
Claim 2
Dependent Claim
55 words
A process for the conversion of triphenylphosphine oxide to triphenylphosphine comprising the steps of (a) reacting triphenylphosphine oxide with a dialkylaluminum hydride of which the alkyl groups are the same or different and each contain from 1 to 15 carbon atoms in a straight or branched chain; and (b) hydrolyzing the product of step (a).
Claim 3
Dependent Claim
37 words
The process of claim 1 in which the alkyl groups in the dialkylaluminum hydride of step (a) are the same or different and each contain from 1 to 5 carbon atoms in a straight or branched chain.
Claim 4
Dependent Claim
16 words
The process of claim 1 in which the dialkylaluminum hydride of step (a) is diisobutylaluminum hydride.
Claim 5
Dependent Claim
20 words
The process of claim 1 in which the reaction of step (a) occurs in the presence of an aliphatic solvent.
Claim 6
Dependent Claim
17 words
The process of claim 4 in which the aliphatic solvent contains 6 to 8 carbon atoms, inclusive.
Claim 7
Dependent Claim
24 words
The process of claim 1 in which the reaction of step (a) occurs at a temperature between about 20° C. and about 140° C.
Claim 8
Dependent Claim
24 words
The process of claim 1 in which the reaction of step (a) occurs at a temperature between about 60° C. and about 130° C.
Claim 9
Dependent Claim
17 words
The process of claim 1 in which the reaction of step (a) occurs at approximately atmospheric pressure.
Claim 10
Dependent Claim
24 words
The process of claim 1 in which the mole ratio of dialkylaluminum hydride to triphenylphosphine oxide in step (a) is greater than about 1.0.
Claim 11
Dependent Claim
26 words
The process of claim 1 in which the mole ratio of dialkylaluminum hydride to triphenylphosphine oxide in step (a) is between about 1.0 and about 5.0.
Claim 12
Dependent Claim
22 words
The process of claim 1 in which step (b) is conducted at a temperature from about -10° C. to about +20° C.
Claim 13
Dependent Claim
24 words
The process of claim 1 in which step (b) is conducted in the presence of a base of pH of at least about 10.
Claim 14
Dependent Claim
15 words
The process of claim 1 in which step (b) is conducted at approximately atmospheric pressure.
Claim 15
Dependent Claim
16 words
The process of claim 1 in which triphenylphosphine is recovered from the product of step (b).
Claim 16
Dependent Claim
23 words
The process of claim 1 in which unreacted triphenylphosphine oxide is separated from the product of step (b) and recycled to step (a).
Claim 17
Dependent Claim
57 words
The process of claim 1 in which the dialkylaluminum hydride of step (a) is generated in situ by heating a trialkyl-aluminum in which one alkyl group contains a minimum of two carbon atoms and a minimum of one hydrogen atom directly bonded to a β-carbon atom, to a temperature between about 50° C. and about 175° C.
Claim 18
Dependent Claim
22 words
The process of claim 16 in which the trialkylaminum is heated to a temperature between about 100° C. and about 150° C.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1981-09-11 | 1982-03-13 | 1982-09-12 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1985-09-11 | 1986-03-13 | 1986-09-12 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1989-09-11 | 1990-03-13 | 1990-09-12 | $7700.00 | Window Closed / Lapsed |