Sulfuric Acid → HCID 12081709, compound

Participants

Reaction Conditions

Reaction Steps

Into a 1 liter four-necked flask equipped with a thermometer, a stirrer and a dropping funnel, 450 ml of ion-exchanged water, 75 ml of a concentrated sulfuric acid and 45.20 g (0.15 moles) of dimethyl 5-(4-aminophenoxy)isophthalate obtained in accordance with the same procedures as those conducted in Example 5 were placed and the resultant mixture was stirred. The flask was cooled at a temperature of 50° C. or lower. Into the cooled flask, a solution prepared by dissolving 12.42 g (0.18 moles) of sodium nitrite into 25 ml of distilled water was added dropwise over 20 minutes. The resultant mixture was stirred at a temperature of 5° C. or lower for 40 minutes and at 100° C. for 2 hours. The formed precipitates were separated by filtration and, after a treatment with active carbon in methanol, recrystallized from methanol. The formed solid substance was separated by filtration and dried at 50° C. for 1 day under a reduced pressure and 23.58 g of a product was obtained (the yield: 52%).

Provenance & Evidence