Yield:78597-27-0 68%

Reaction Conditions:

with iron at 90; for 12 h;

Steps:

12.a a) 5-lodo- 1H-benzo[djimidazole
Intermediate Example 12.5-((Trimethylsilyl)ethynyl)- 1H-benzo[d]imidazolea) 5-lodo- 1H-benzo[djimidazoleTo a solution 4-ioclo-2-nitroaniline (1 g, 3.7mmol) in formic acid (10 ml), iron(2.1 g, 37 mmol) was added and heated at 90°C for 12 h. The formic acid was distilledoff and the crude was dissolved in ethyl acetate. The ethyl acetate layer was washed with water, brine and dried over sQdiurn sulphate. The solvent was distilled off to afford the title product in 68 %. yield (0.85 g)..LC-MS (ES]): Calculated mass: 243.95; Observed mass: 244.8 [M+H} + (rt: 0.173 mm).

References:

ORION CORPORATION;RAJAGOPALAN, Srinivasan;APPUKUTTAN, Prasad;NARASINGAPURAM ARUMUGAM, Karthikeyan;UJJINAMATADA, Ravi Kotrabasaiah;GEORGE, Shyla;LINNANEN, Tero WO2014/162039, 2014, A1 Location in patent:Page/Page column 39

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