4,5-Dibromo-1-methyl-2-trichloroacetylpyrrole Ⅰ, prepared by the reaction of 1-methyl-2-trichloroacetylpyrrole with Br2 in 98.6 % yield, was condensed with methyl L-2-amino-3- phenylpropanoate to afford methyl 2-(4,...4,5-Dibromo-1-methyl-2-trichloroacetylpyrrole Ⅰ, prepared by the reaction of 1-methyl-2-trichloroacetylpyrrole with Br2 in 98.6 % yield, was condensed with methyl L-2-amino-3- phenylpropanoate to afford methyl 2-(4,5-dibromo-1-methylpyrrole-2-carboxmido)-3-phenylpropanoate Ⅱ in 90.8% yield. Crystal data for Ⅰ: monoclinic system, space group P21/c with a = 8.595(3), b = 10.900(4), c = 12.321(5) ,A°,β = 92.292(7)°, V = 1153.4(8)A°^3, Dc = 2.213 g/cm^3, F(000) = 728, CTH4Br2Cl3NO, Mr = 384.28, λ = 0.71073 A°, μ(MoKa) = 7.688 mm^-1, Z = 4, R = 0.0338 and wR2 = 0.0840 for 1963 observed reflections with I 〉 2a(I). Crystal data for Ⅱ: monoclinic system, space group P21 with a = 4.886(2), b = 15.921(8), c = 11.635(6) A°,β = 101.803(9)°, V = 885.9(7) A°^3, Dc = 1.665 g/cm^3, F(000) = 440, C16H16Br2N2O3, Mr = 444.13, λ = 0.71073 A°, μ(MoKa) = 4.590 mm^-1, Z = 2, R = 0.0335 and wR2 = 0.0837 for 3191 observed reflections with I 〉 2σ(I). The crystal structure reveals that compound Ⅱ forms the one-dimensional chain structure via the intermolecular hydrogen bonds of N(2)-H…O(1).展开更多
A new halogenated biindole and a new apo-carotenone have been isolated from the ethanolic extract of the green alga Chaetomorpha basiretorsa Sethcell. On the basis of chemical and spectroscopic methods including 2D NM...A new halogenated biindole and a new apo-carotenone have been isolated from the ethanolic extract of the green alga Chaetomorpha basiretorsa Sethcell. On the basis of chemical and spectroscopic methods including 2D NMR technique, their structures have been elucidated as 4,4′-dichloro-5,5′-dibromo-7,7′-dimethoxy-2,2′-bi-1H-indole and 1′S*,4′R*-8-(4′-hydroxy-2′,6′,6′- trimethylcyclohex-2-enyl)-6-methyloct-3E,5E,7E-trien-2-one, respectively.展开更多
基金The project was supported by the National 863 Program of China (No. 2004AA628030), and Natural Science Foundation of Guangdong Province (No. 31920)
文摘4,5-Dibromo-1-methyl-2-trichloroacetylpyrrole Ⅰ, prepared by the reaction of 1-methyl-2-trichloroacetylpyrrole with Br2 in 98.6 % yield, was condensed with methyl L-2-amino-3- phenylpropanoate to afford methyl 2-(4,5-dibromo-1-methylpyrrole-2-carboxmido)-3-phenylpropanoate Ⅱ in 90.8% yield. Crystal data for Ⅰ: monoclinic system, space group P21/c with a = 8.595(3), b = 10.900(4), c = 12.321(5) ,A°,β = 92.292(7)°, V = 1153.4(8)A°^3, Dc = 2.213 g/cm^3, F(000) = 728, CTH4Br2Cl3NO, Mr = 384.28, λ = 0.71073 A°, μ(MoKa) = 7.688 mm^-1, Z = 4, R = 0.0338 and wR2 = 0.0840 for 1963 observed reflections with I 〉 2a(I). Crystal data for Ⅱ: monoclinic system, space group P21 with a = 4.886(2), b = 15.921(8), c = 11.635(6) A°,β = 101.803(9)°, V = 885.9(7) A°^3, Dc = 1.665 g/cm^3, F(000) = 440, C16H16Br2N2O3, Mr = 444.13, λ = 0.71073 A°, μ(MoKa) = 4.590 mm^-1, Z = 2, R = 0.0335 and wR2 = 0.0837 for 3191 observed reflections with I 〉 2σ(I). The crystal structure reveals that compound Ⅱ forms the one-dimensional chain structure via the intermolecular hydrogen bonds of N(2)-H…O(1).
基金supported by national 863 project(Grant No.2004AA625030,2001AA620503)NNSFC(Grant No.20432030)Key Innovative Project of the Academy(Grant No.KZCX3-SW-215).
文摘A new halogenated biindole and a new apo-carotenone have been isolated from the ethanolic extract of the green alga Chaetomorpha basiretorsa Sethcell. On the basis of chemical and spectroscopic methods including 2D NMR technique, their structures have been elucidated as 4,4′-dichloro-5,5′-dibromo-7,7′-dimethoxy-2,2′-bi-1H-indole and 1′S*,4′R*-8-(4′-hydroxy-2′,6′,6′- trimethylcyclohex-2-enyl)-6-methyloct-3E,5E,7E-trien-2-one, respectively.