تفاعل #1721

معادلة التفاعل

4-phenoxybenzonitrile

dibutyltin oxide

trimethylsilyl azide

→

5-(4-phenoxyphenyl)-1H-tetrazole

المذيبات

toluene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةto reflux for 6 hours
2. 2
   غسيلThe reaction mixture was washed with 1.6M sodium hydroxide (2×250 ml)
3. 3
   غسيلThe combined aqueous layer was washed with diethyl ether (4×120 ml)
4. 4
   غسيلThe acidic solution was washed with ethyl acetate (3×200 ml)
5. 5
   تجفيفthe combined organic layer was dried over anhydrous sodium sulfate
6. 6
   ترشيحfiltered
7. 7
   أخرىevaporated to dryness

الإجراء التجريبي

A solution of 4-phenoxybenzonitrile (9.87 g), dibutyltin oxide (3.88 g), and trimethylsilyl azide (33.5 ml) in anhydrous toluene (200 ml) was heated to reflux for 6 hours. The reaction mixture was washed with 1.6M sodium hydroxide (2×250 ml). The combined aqueous layer was washed with diethyl ether (4×120 ml) then acidified to pH 6 with concentrated hydrochloric acid. The acidic solution was washed with ethyl acetate (3×200 ml) and the combined organic layer was dried over anhydrous sodium sulfate, filtered and evaporated to dryness to give 5-(4-phenoxyphenyl)-1H-tetrazole as a white powder.

المصدر