Dimethylformamide → HCID 15570210, compound

Participants

Reaction Conditions

Reaction Steps

Potassium carbonate (177 mg, 1.28 mmol), DMF (2 mL) and MeI (60 μL) were added to the compound (230 mg, 0.65 mmol) obtained in step 1, and stirred at 40° C. for 6 hours. Potassium carbonate (44.3 mg) and MeI (40 μL) were further added thereto and stirred overnight. After removing a solvent, purification was conducted in accordance with the purification process A to obtain a crude product (160 mg) of 3-{methyl[(2-nitrophenyl)sulfonyl]amino}benzenesulfonic acid. The crude product (144 mg, 0.39 mmol) was dissolved in DMF (3 mL), and cesium carbonate (126 mg, 0.39 mmol) and thiophenol (40 μL, 0.39 mmol) were added thereto and stirred at 50° C. overnight. After removing a solvent, purification was conducted in accordance with the purification process A to obtain to a crude product (84.1 mg) of 3-(methylamino)benzenesulfonic acid. Then, a title compound was obtained by the same method as that of the synthetic example 1 except that the crude product of 3-(methylamino)benzenesulfonic acid was used instead of 3-sulfoaniline.

Provenance & Evidence