US5756724A
Expired / Lapsed
US
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High-yielding ullmann reaction for the preparation of bipyrroles
Assignee: Cytopharm Inc
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Filing: 1997-04-22
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Granted: 1998-05-26
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Expires: 2017-04-22
Abstract
Abstract Coupling two moles of a 2-halopyrrole in the presence of an inert aromatic solvent and a catalytically effective amount of a substantially pure copper catalyst provides high yields of the corresponding bipyrrole.
Inventors
- 👤 Emanuel Vogel
- 👤 Reiner Deponte
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-09 03:32
CPC Classifications
C; C07; C07D; C07D207/00; C07D207/02; C07D207/30; C07D207/34
Claims Analysis
Total Claims: 17
Claim 1
Independent Claim
130 words
A method of preparing a bipyrrole, comprising the step of: heating a 2-halopyrrole of the formula ##STR6## wherein X is a halogen; R 1 is hydrogen or a group of the formula C(O)--OR 5 where R 5 is an alkyl, arylalkyl or aryl group; R 2 is a group of the formula C(O)--OR 5 where R 5 is as described above; R 3 and R 4 are, independently, hydrogen, alkyl, alkoxyalkyl or a group of the formula C(O)--OR 5 where R 5 is as described above; in the presence of an inert aromatic solvent and a catalytically effective amount of a substantially pure copper catalyst to form a bipyrrole of the formula ##STR7## wherein R 1 , R 2 , R 3 , and R 4 are as described above.
Claim 2
Independent Claim
130 words
A method of preparing a bipyrrole, comprising the step of: heating a 2-halopyrrole of the formula ##STR6## wherein X is a halogen; R 1 is hydrogen or a group of the formula C(O)--OR 5 where R 5 is an alkyl, arylalkyl or aryl group; R 2 is a group of the formula C(O)--OR 5 where R 5 is as described above; R 3 and R 4 are, independently, hydrogen, alkyl, alkoxyalkyl or a group of the formula C(O)--OR 5 where R 5 is as described above; in the presence of an inert aromatic solvent and a catalytically effective amount of a substantially pure copper catalyst to form a bipyrrole of the formula ##STR7## wherein R 1 , R 2 , R 3 , and R 4 are as described above.
Claim 3
Dependent Claim
9 words
The method of claim 1, wherein X is I.
Claim 4
Dependent Claim
10 words
The method of claim 1, wherein R 1 is H.
Claim 5
Dependent Claim
19 words
The method of claim 1, wherein R 1 is C (O)--OR 5 and R 5 is C 1-10 alkyl.
Claim 6
Dependent Claim
15 words
The method of claim 1, wherein R 3 and R 4 are C 1-10 alkyl.
Claim 7
Dependent Claim
17 words
The method of claim 1, wherein R 3 is C 1-10 alkyl and R 4 is hydrogen.
Claim 8
Dependent Claim
19 words
The method of claim 1, wherein R 3 is C 1-10 alkoxy-C 1-10 alkyl and R 4 is hydrogen.
Claim 9
Dependent Claim
17 words
The method of claim 1, wherein said inert aromatic solvent is a C 6-20 aromatic hydrocarbon solvent.
Claim 10
Dependent Claim
16 words
The method of claim 8, wherein said heating is conducted at a temperature of 75°-250° C.
Claim 11
Dependent Claim
16 words
The method of claim 9, wherein said heating is conducted at a temperature of 100°-200° C.
Claim 12
Dependent Claim
33 words
The method of claim 1, wherein R 1 is C(O)--OR 5 , R 3 is C 1-10 alkyl or C 1-10 alkoxy-C 1-10 alkyl, R 4 is C(O)--OR 5 and X is I.
Claim 13
Dependent Claim
26 words
The method of claim 1, wherein R 1 is hydrogen, R 3 is C 1-10 alkoxy-C 1-10 alkyl, R 4 is hydrogen and X is I.
Claim 14
Dependent Claim
55 words
The method of claim 1, wherein R 1 is H, further comprising reacting said bipyrrole with a formylating agent to form a bipyrrole dialdehyde of the formula ##STR8## wherein R 3 is C 1-10 alkyl or C 1-10 alkoxy-C 1-10 alkyl and R 4 is hydrogen, C 1-10 alkyl or C 1-10 alkoxy-C 1-10 alkyl.
Claim 15
Dependent Claim
14 words
The method of claim 13, wherein said formylating agent is POCl 3 and dimethylformamide.
Claim 16
Dependent Claim
40 words
The method of claim 13, further comprising coupling two moles of said bipyrrole dialdehyde to form a porphycene having the formula ##STR9## wherein R 3 and R 4 are, independently, hydrogen, C 1-10 alkyl or C 1-10 alkoxy-C 1-10 alkyl.
Claim 17
Dependent Claim
20 words
The method of claim 15, wherein said coupling is conducted in the presence of Ti +2 or Ti +3 .
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 2001-05-25 | 2001-11-24 | 2002-05-26 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2005-05-25 | 2005-11-24 | 2006-05-26 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2009-05-25 | 2009-11-24 | 2010-05-26 | $7700.00 | Window Closed / Lapsed |