反应详情

To a mixture (4-Amino-phenoxy)acetic acid HCl 60 (250 grams, 1.228 mol), in methanol (5 liters) was passed dry HCl gas at 10° C. for 1 hour and refluxed for 10 hours. Methanol (3.5 liters) was distilled and ice water (1 liter) was added and the pH was adjusted to 7.5 with K2CO3. Crude 61 was filtered, dried, and recrystallized from a mixture of Chloroform:Hexane (1:5) to give pure 61 (130 grams, 58.5%) as a light brown powder The melting point was found to be 65-66.8° C.

1. customat 10° C.
2. customfor 1 hour
3. temperaturerefluxed for 10 hours
4. distillationMethanol (3.5 liters) was distilled
5. additionice water (1 liter) was added
6. filtrationCrude 61 was filtered
7. customdried
8. customrecrystallized from a mixture of Chloroform:Hexane (1:5)