Chiral salen catalyst and methods for prepn. of chirol compounds from racemic epoxides by using new catalyst
A technology for chiral compounds and catalysts, applied in chemical instruments and methods, organic chemistry methods, cobalt organic compounds, etc., can solve problems such as restrictions on reuse and increase the manufacturing price of chiral epoxides
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Embodiment 1
[0062] Hereinafter, the present invention will be described in more detail using examples. However, this should not be construed as limiting the scope of the invention. Embodiment 1: the preparation of I-SS-1
[0063] Mix 1 equivalent of (S,S)-N,N'-bis(3,5-di-tert-butylsalicylidene)-1,2-cyclohexanediamine and 1.2 equivalents of cobalt acetate in ethanol (II) 4H 2 O, and reflux for 5 hours with stirring. The reaction mixture was filtered and washed with a small amount of ethanol. The obtained solid was mixed with 0.5 equivalent of boron trifluoride·2H 2 O was mixed in dichloromethane and the reaction mixture was stirred at room temperature for 4 hours. Dichloromethane was removed under reduced pressure to yield the desired compound.
[0064] IR 70, 1010, 1070, 1100, 1220, 1270, 1360, 1560, 1720cm -1 ;
[0065] UV / visible light 360nm;
[0066] 13 C NMR (CDCl 3 , ppm) δ17.62, 22.33, 24.42, 29.57, 31.51, 32.34, 33.70, 42.93, 47.03, 56.53, 82.37, 92.93, 97.47, 126.18; ...
Embodiment 2
[0069] Analysis calculation (C 72 h 104 N 4 o 4 co 2 ·BF 3 ·3H 2 O) C 65.1, H 8.3, N 4.2, found C 65.4, H 8.5, N 4.2. Embodiment 2: Preparation of I-RR-1 a) Except that (S,S)-N,N'-bis(3,5-di-tert-butylsalicylidene)-1,2-cyclohexanediamine is replaced by
[0070] (R, R)-N, N'-bis(3,5-di-tert-butylsalicylidene)-1,2-cyclohexanediamine, using the above
[0071] The same method in Example 1 was used to obtain the target product.
[0072] IR 970, 1010, 1070, 1100, 1220, 1270, 1360, 1560, 1720cm -1 ;
[0073] UV / visible light 360nm;
[0074] 13 C NMR (CDCl 3 , ppm) δ 17.62, 22.33, 24.42, 29.57, 31.51, 32.34, 33.70, 42.93, 47.03, 56.53, 82.37, 92.93, 97.47, 126.18;
[0075] 19 F NMR (CDCl 3 )(CFCl 3 , ppm) δ-87.62;
[0076] 11 B NMR (CDCl 3 )(BF 3 , ppm) δ0.31; and
[0077] Analysis calculation (C 72 h 104 N 4 o 4 co 2 ·BF 3 ·3H 2 O) C 65.1, H 8.3, N 4.2, found C 65.4, H 8.5, N 4.2. b) Except that (S,S)-N,N'-bis(3,5-di-tert-butylsalicylidene)-1,2-cyclohex...
Embodiment 3
[0083] The target product was obtained in the same manner as in Example 1 above. Embodiment 3: the preparation of I-SS-2
[0084] Except replacing (S,S)-N,N'-bis(3,5-di-tert-butylsalicylidene)-1,2-cyclohexanediamine with (S)-N-(3, 5-di-tert-butyl salicylidene)-(S)-N'(salicylidene)-1,2-cyclohexanediamine, using the same method as in Example 1 above to obtain the desired product .
[0085] IR 970, 1010, 1070, 1100, 1220, 1270, 1360, 1560, 1720cm -1 ;and
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