IPC분류정보
국가/구분 |
United States(US) Patent
등록
|
국제특허분류(IPC7판) |
|
출원번호 |
US-0312999
(2001-06-26)
|
우선권정보 |
EP-0810589 (2000-07-05) |
국제출원번호 |
PCT/EP01/07265
(2001-06-26)
|
국제공개번호 |
WO02/02571
(2002-01-10)
|
발명자
/ 주소 |
- Beck, Gerhard
- Korhummel, Claus
- Baier, Hanspeter
- Bachmann, Frank
- Makowka, Cornelia
- Linde, Reiner
- Kirrmann, Bernd
|
출원인 / 주소 |
- Ciba Specialty Chemicals Corporation
|
대리인 / 주소 |
|
인용정보 |
피인용 횟수 :
2 인용 특허 :
0 |
초록
▼
A process for the preparation of manganese complexes of salen compounds which comprises carrying out the reaction of a salen compound with a manganese compound in DMF is described. In a preferred embodiment, the salen compound itself is synthesised likewise in DMF and reacted without intermediate is
A process for the preparation of manganese complexes of salen compounds which comprises carrying out the reaction of a salen compound with a manganese compound in DMF is described. In a preferred embodiment, the salen compound itself is synthesised likewise in DMF and reacted without intermediate isolation to form the manganese complex.
대표청구항
▼
1. A process for the preparation of a manganese complex of salen compounds of formulain which formulaeA is an anion;n, m and p are each independently of the others 0, 1, 2 or 3,R, R 1 and R 1 ′ are each independently of the others cyano; halogen; OR 4 or COOR 4 , wherein R 4 is hydrogen
1. A process for the preparation of a manganese complex of salen compounds of formulain which formulaeA is an anion;n, m and p are each independently of the others 0, 1, 2 or 3,R, R 1 and R 1 ′ are each independently of the others cyano; halogen; OR 4 or COOR 4 , wherein R 4 is hydrogen or linear or branched C 1 -C 4 alkyl; nitro; linear or branched C 1 -C 8 alkyl; linear or branched partially fluorinated or pertfluorinated C 1 -C 8 alkyl; NR 5 R 6 , wherein R 5 and R 6 are identical or different and are each independently of the other hydrogen or linear or branched C 1 -C 12 alkyl; or linear or branched C 1 -C 8 alkyl-R 7 , wherein R 7 is a radical NH 2 , OR 4 , COOR 4 or NR 5 R 6 as defined above; or -CH 2 —N ⊕ R 4 R 6 R 7 or —N ⊕ R 4 R 5 R 8 , wherein R. 4 , R 5 and R 6 are as defined above,R 2 and R 3 are each independently of the other hydrogen, linear or branched C 1 -C 4 alkyl or unsubstituted aryl or aryl that is substituted by cyano; by halogen; by OR 4 or COOR 4 , wherein R 4 is hydrogen or linear or branched C 1 -C 4 alkyl; by nitro; by linear or branched C 1 -C 8 alkyl; by NHR 5 or NR 5 R 6 , wherein R 5 and R 6 are identical or different and are each hydrogen or linear or branched C 1 -C 12 alkyl or wherein R 5 and R 6 together with the nitrogen atom linking them form a 5-, 6- or 7-membered ring that may contain further hetero atoms; or by linear or branched C 1 -C 8 alkyl-R 7 , wherein R 7 is a radical NH 2 , OR 4 , COOR 4 or NR 5 R 6 as defined above; or by —N ⊕ R 4 R 5 R 6 , wherein R 4 , R 5 and R 6 are as defined above,R 8 radicals are each independently of the others hydrogen or linear or branched C 1 -C 4 alkyl,Y is a linear or branched alkylene radical of formula —[C(R 4 ) 2 ] r —, wherein r is an integer from 1 to 8 and the R 4 radicals are each independently of any other(s) as defined above; —CX═CX—, wherein X is cyano, linear or branched C 1 -C 8 alkyl or di(linear or branched C 1 -C 8 alkyl)amino;—(CH 2 ) q —NR 4 —(CH 2 ) q —, wherein R 4 is as defined above and q is 1, 2, 3 or 4; or a 1,2-cyclohexylene radical of formula:wherein R 9 is hydrogen, SO 3 H, CH 2 OH or CH 2 NH 2 ,wherein in formula (1) the phenyl rings may together carry no more than three tert-butyl substituents, and wherein, when Y is 2-hydroxypropylene and m and n are each 0, R 2 and R 3 may not both be H,which comprises reacting a ligand of formulawherein R, R 1 , R 1 ′, R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R 8 , R 9 , Y, A, n, m and p are as defined for formulae (1), (2) and (3),with a manganese(II) salt in dimethylformamide as solvent. 2. A process according to claim 1, wherein the synthesis of the ligand and the reaction to form the manganese complex are carried out in dimethylformamide in a one-pot reaction. 3. A process according to claim 1, which comprises reacting, in dimethylformamide as solvent, a diamine of formula 2 N—Y—NH 2 (7)with an o-hydroxybenzaldehyde of formulaor reacting the compound of formula 2 —CH 2 —NH 2 ) 3 (10)with an o-hydroxybenzaldehyde of formula (8), in which formulae Y, R, R 2 , R 9 and n are as defined for formulae (1) and (2) in claim 1, and then, without intermediate isolation, reacting the resulting salen compound with a manganese(II) salt to form a manganese complex of formula (1), (2) or (3). 4. A process according to claim 1, wherein Y is a radical of formula —(CH 2 ) r — wherein r is an integer from 1 to 8, or a radical of formula —C(R 5 ) 2 —(CH 2 ) p —C(R 5 ) 2 — wherein p is a number from 0 to 6 and R 5 is hydrogen or C 1 -C 4 alkyl. 5. A process according to claim 1, wherein R, R 1 and R 1 ′ are hydrogen, nitro, OR 4 , COOR 4 or N(R 4 ) 2 , wherein R 4 is hydrogen or C 1 -C 4 alkyl. 6. A process according to claim 1, wherein R 2 and R 3 are hydrogen, methyl, ethyl or unsubstituted phenyl. 7. A process according to claim 1, which is carried out at a temperature of from approximately 20 to 70° C. 8. A process according to claim 1, wherein the manganese compound is added in an excess of from 0.5 to 3%. 9. A process according to claim 3, wherein the first reaction is carried out at approximately from 10 to 40° C., and the di- or tri-amine and aldehyde are used approximately in a molar ratio of 1:2 or 1:3.
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