反应详情

A 350 ml three necked reaction flask, equipped with a mechanical stirrer, a thermometer a “wood metal” heating bath and a reflux condenser combined with a water separator were charged with 25.1 g (140 mmol) of 2-amino-4-(1,1-dimethyl-propyl)-phenol (see above), 19.3 g (140 mmol) of 4-hydroxy benzoic acid and 1.5 g of boric acid suspended in 140 ml of 1,2-dichlorobenzene under nitrogen atmosphere. This mixture was refluxed until two equivalents of water had separated (about 4 hours). When cold, 50 ml of diisopropylether were added and this mixture was filtered and the crystalline product was washed with diisopropylether and pentane and dried. 32.1 g (81%) of the product were obtained. M.p. 236-237° C.

1. temperaturea thermometer a “wood metal” heating bath and a reflux condenser
2. customhad separated (about 4 hours)
3. additionWhen cold, 50 ml of diisopropylether were added
4. filtrationthis mixture was filtered
5. washthe crystalline product was washed with diisopropylether and pentane
6. customdried