【摘 要】
:
The intermediate of d-biotin, (3aS,6aR)-1,3-dibenzyltetrahydro-1H-thieno[3,4-d]-imidazole-2(3H)-one-4-ylidenepentanoil acid was synthesized from (3aS,6aR)-1,3-d
【机 构】
:
Department of Chemistry,Research Center for Analysis and Measurement
论文部分内容阅读
The intermediate of d-biotin, (3aS,6aR)-1,3-dibenzyltetrahydro-1H-thieno[3,4-d]-imidazole-2(3H)-one-4-ylidenepentanoil acid was synthesized from (3aS,6aR)-1,3-dibenzyltetrahyro4H-thieno[3,4-d]-imidazole-2,4(1H)-dione by using the Grignard reaction. The structure of 3 was characterized by IR, 1H NMR and MS, and the absolute configuration was further confirmed by X-ray crystal structure analysis. Compound 3 crystallizes in monoclinic, space group P21 with a = 11.030(2), b = 7.783(2), c = 12.797(2)A, β = 93.44(1)°, Z = 2, Mr = 422.53 (C24H26N2O3S), V =1096.3(6)A3, μ = 0.177 mm-1, Dc = 1.280 g/cm3, F(000) = 448 and T= 293(2) K. The final R =0.0737 and Rw = 0.1974 for 1009 observed reflections with I >2σ(I).
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