تفاعل #2254230

معادلة التفاعل

5-fluoro-2-nitro-benzaldehyde

butanol

→

desired compound

المردود 192.0%

2-Dibutoxymethyl-4-fluoro-1-nitro-benzene

المردود 192.0%

المذيبات

ethyl acetate

toluene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةat reflux for 2 hours in a flask
2. 2
   أخرىequipped with a Dean-Stark trap
3. 3
   غسيلwash sequentially with saturated aqueous sodium bicarbonate (300 mL×3) and saturated aqueous sodium chloride (300 mL×2)
4. 4
   تجفيفDry the organic phase over sodium sulfate
5. 5
   تركيزconcentrate under reduced pressure

الإجراء التجريبي

Heat a solution of 5-fluoro-2-nitro-benzaldehyde (10 g, 59.17 mmol), butanol (20 mL, 219 mmol) and p-toluenesulfonic acid (600 mg, 3.15 mmol) in toluene (200 mL) at reflux for 2 hours in a flask equipped with a Dean-Stark trap. Cool the reaction mixture to room temperature, dilute with ethyl acetate (400 mL), and wash sequentially with saturated aqueous sodium bicarbonate (300 mL×3) and saturated aqueous sodium chloride (300 mL×2). Dry the organic phase over sodium sulfate and concentrate under reduced pressure to provide the desired compound as a pale yellow oil (17 g, 96%).

المصدر