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0012080295
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note
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Method of Synthesis of Co(II)Salen: In 50 mL of 95% boiling EtOH 4.9 g (40 mmol) of salicylaldehyde was dissolved. To this solution 1.2 g (20 mmol) of ethylenediamine was added dropwise. The reaction was stirred for 3.5 h. After completion, the reaction mixture was cooled. N,N′-Bis(salicylidene)ethylenediimine yellow crystals were precipitated, filtered out, washed with 20 mL of EtOH and finally dried. Subsequently, 2 g (7.45 mmol) of Schiff base was dissolved in 120 mL of EtOH. The reaction was carried out under argon atmosphere. The cobalt(II) acetate 1.85 g (8.37 mmol) solution in 15 mL of warm water (60°C) was added dropwise. A brown-red gelatinous product was formed, which next changed to red crystals. The reaction was stirred for 1 h. After cooling, the crystals of Co(II)Salen complex were filtered and dried at 60°C (under vacuum) overnight.
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17
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0012017837
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3 solution for 6 h. Deprotonated polymer was dried at 60°C for 24 h and washed again with water and MeOH. All these purification steps are important for the entire removal of all oligomeric species accompanying the polymer.
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0012017838
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(a) Preparation of Polyaniline Supported Cobalt(II) Acetate is Representative for the Procedure Employed for Cobalt(II) Acetate Based Catalysts: A mixture of polyaniline (500 mg) and cobalt acetate (500 mg) was stirred in an MeCN (25 mL) and HOAc (25 mL) mixture for 72 h at r.t. Then the reaction mixture was filtered and the solid catalyst was washed with MeCN (5 × 5 mL). The catalyst was dried at 110°C for 24 h.
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0012080297
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(b) Preparation of Polyaniline Supported Co(II)Salen is Representative for the Procedure Employed for Co(II)Salen Based Catalysts: A mixture of polyaniline (500 mg) and Co(II)Salen (500 mg) was stirred in 50 mL of MeCN for 48 h at r.t. The reaction mixture was filtered and the solid catalyst was stirred again with 50 mL of HOAc for 1 h at r.t. The reaction mixture was filtered and the solid filtrate was first washed with HOAc (3 × 10 mL) and then MeCN (5 × 5 mL). The catalyst was dried at 110°C for 24 h.
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20
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0012046403
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4 and the evaporation of solvent yielded the desired product, which was purified by Kugelrohr distillation.
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Yamada, T.; Imagawa, K.; Nagata, T.; Mukaiyama, T. Chem. Lett. 1992, 11, 2231.
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(1992)
Chem. Lett.
, vol.11
, pp. 2231
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Yamada, T.1
Imagawa, K.2
Nagata, T.3
Mukaiyama, T.4
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