Dimethylformamide → HCID 86688836, compound

Participants

Reaction Steps

To a solution of benzothiophenobenzothiophene 20 (300 mg, 0.58 mmol) in 7 ml of dichloromethane is added a solution of 1.1 ml (11.4 mmol) of phosphorus oxychloride and 0.94 ml (12.2 mmol) of DMF in 7 ml of DCM. The reaction mixture is refluxed for 16 h, then sat. sodium hydrogencarbonate solution (50 ml) is added and the mixture is stirred at room temperature for 2 h. After phase separation, the organic phase is dried over sodium sulfate. After the solvents have been distilled off, the residue is recrystallized from toluene to obtain 172 mg (52%) of product. 1H NMR (TCE-d2, 375 K): 9.83 ppm (s, 2H), 8.01 (d, 2H), 7.90 (s, 2H), 7.61 (s, 4H), 2.92 (dd, 4H), 1.72 (m, 4H), 1.44 (qa, 4H), 0.95 (t, 6H).

Provenance & Evidence