2,4-DIAMINO-PHENOL

In the reaction flask, M-3 (5 g, 0.035 mol), 2-Bromopropane (5.5g, 0 · 045mol), potassium carbonate (6.2g, 0.045mol), potassium iodide (0.12g, 0.0007mol), DMF (30ml), reacted at 60 C for 3h, monitored by TLC, after the reaction is completed, cooled to room temperature, the reaction solution was poured into water, a large amount of solids were precipitated, stirred for 30 min, pumped Filter, filter cake washed, dried, The obtained crude product was recrystallized from ethanol to give 5 g of white solid, yield: 77.9%.General procedure: A solution of 12 (50mmol), anhydrous potassium carbonate (65mmol), potassium iodide (1mmol), and alkyl halide (75mmol) in DMF (40mL) was stirred at 50C for 6h under nitrogen atmosphere. After the reaction was completed, the mixture was poured into water (200mL). Then the precipitate was filtered and recrystallized from ethanol to yield 4-alkoxy- isophthalonitrile (13a-l).General procedure: A solution of 12 (50mmol), anhydrous potassium carbonate (65mmol), potassium iodide (1mmol), and alkyl halide (75mmol) in DMF (40mL) was stirred at 50C for 6h under nitrogen atmosphere. After the reaction was completed, the mixture was poured into water (200mL). Then the precipitate was filtered and recrystallized from ethanol to yield 4-alkoxy- isophthalonitrile (13a-l).General procedure: A solution of 12 (50mmol), anhydrous potassium carbonate (65mmol), potassium iodide (1mmol), and alkyl halide (75mmol) in DMF (40mL) was stirred at 50C for 6h under nitrogen atmosphere. After the reaction was completed, the mixture was poured into water (200mL). Then the precipitate was filtered and recrystallized from ethanol to yield 4-alkoxy- isophthalonitrile (13a-l).General procedure: A solution of 12 (50mmol), anhydrous potassium carbonate (65mmol), potassium iodide (1mmol), and alkyl halide (75mmol) in DMF (40mL) was stirred at 50C for 6h under nitrogen atmosphere. After the reaction was completed, the mixture was poured into water (200mL). Then the precipitate was filtered and recrystallized from ethanol to yield 4-alkoxy- isophthalonitrile (13a-l).