反応 #159254

反応方程式

water

water

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

4-hydroxy benzoic acid

boric acid

→

product

収率 81.5%

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

収率 81.5%

溶媒

1,2-dichlorobenzene

反応条件

後処理

1. 1
   温度a thermometer a “wood metal” heating bath and a reflux condenser
2. 2
   その他had separated (about 4 hours)
3. 3
   workup.ADDITIONWhen cold, 50 ml of diisopropylether were added
4. 4
   ろ過this mixture was filtered
5. 5
   洗浄the crystalline product was washed with diisopropylether and pentane
6. 6
   その他dried

実験手順

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.

出典