Sodium dithionite-initiated reactions of pyrrole and 1methylpyrrole with 1-bromo-1-chloro-2,2,2-ethane in an acetonitrile-water mixture provide the respective 5-(trifluoromethyl)dipyrromethanes 1 and 3 as main products in 40-58% isolated yields and of high purity. Small amounts of tripyrranes 2 and 4 are also formed and could be isolated from the reaction mixtures. 1-Methyl-2,5-bis[2,2,2-trifluoro-1-(1-methyl-2-pyrrolo)ethyl]pyrrole (4) Mp 194-196 °C. EI-MS: m/z (%) = 403 (58, M + ), 334 [100, (M -CF 3 ) + ], 265 [33, (M -2CF 3 ) + ], 162 (8), 133 (26), 94 (15). Crystal Structure of 3 Molecular Formula: C 12 H 13 F 3 N 2 , F.W. = 242.24. X-Ray diffraction experiment was performed on a Nonius BV MACH3 diffractometer using graphite monochromatised CuKa radiation (l = 1.54178 Å). Lattice constants for compound 3 were determined by a least squares fit of the setting angles of 15 reflections: a = 8.8547(6), b = 8.5247(4), c = 15.4952(9) Å, b = 91.644(5) o , V = 1169.15(12) Å 3 , Z = 4, D c = 1.376 Mgm -3 , monoclinic space group P2 1 /n, F(000) = 504, absorption coefficient m(CuKa) = 1.002 mm -1 , crystal size 0.56´0.35´0.35 mm. 1632 Unique reflections have been masured in the q-range 5.69 to 73.97 o . These have been corrected for LP and y-scan based absorption (max. and min. transmission

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