Potassium Iodide → HCID 15476351, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 2-(9,9-diethyl-7-bromo-2-) fluorenyl benzothiazole, (6.6 g., 0.015 mol.), potassium carbonate (10.3 g.,0.0746 mol.), diphenylamine (4.5 g. 0.0376 mol.), potassium iodide (9.6 g. 0.0173 mol.), copper bronze (2.0 g., 0.0317 mol.), copper (I) iodide (1.5 g., 0.0079 mol.), 18-crown-6 (0.96 g., 0.0036 mol.), and 1,2-dichlorobenzene (45 ml.) was kept at 180-1820° C. for 20 hours, cooled and filtered. The filtrate was concentrated and the residue was transferred to a column of silica gel. Elution with heptane gave the product, 3.6 g.(45.5% yield), m.p. 175-178.4° C. Recrystallization from 9:1 heptane-toluene raised the m.p. to 178-180° C. Mass Spec: (m/z) 522, (M+). Anal. Calcd. for C36H30N2S: C, 82.76; H, 5.79; N, 5.36; and S, 6.12. Found: C, 82.41; H, 5.52; N, 5.25; and S, 5.99.

Provenance & Evidence