Reaktion #159254

Reaktionsgleichung

water

water

2-amino-4-(1,1-dimethyl-propyl)-phenol

4-hydroxy benzoic acid

boric acid

→

product

Ausbeute 81.5%

4-[5-(1,1-Dimethyl-propyl)-benzooxazol-2-yl]-phenol

Ausbeute 81.5%

Lösungsmittel

1,2-dichlorobenzene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperatura thermometer a “wood metal” heating bath and a reflux condenser
2. 2
   Sonstigehad separated (about 4 hours)
3. 3
   workup.ADDITIONWhen cold, 50 ml of diisopropylether were added
4. 4
   Filtrationthis mixture was filtered
5. 5
   Waschenthe crystalline product was washed with diisopropylether and pentane
6. 6
   Sonstigedried

Vorschrift

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.

Quelle