تفاعل #63297

معادلة التفاعل

2,2,3,3,4,4,4-heptafluoro-N-[2-(cyanomethyl)phenyl]butanamide

sodium azide

ammonium chloride

dimethylformamide

→

title compound

المردود 18.9%

2,2,3,3,4,4,4-Heptafluoro-N-[2-(1H-tetrazol-5-ylmethyl)phenyl]butanamide

المردود 18.9%

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe reaction mixture was cooled to room temperature
2. 2
   استخلاصthe product was extracted with ethylacetate (3×200 mL)
3. 3
   تجفيفThe combined extracts were dried over Na2SO4
4. 4
   ترشيحfiltered
5. 5
   تركيزconcentrated with a rotary evaporator
6. 6
   أخرىThe brown residue was purified by high pressure liquid chromatography
7. 7
   أخرىto give a white solid
8. 8
   أخرىThe solid was triturated with diethyl ether

الإجراء التجريبي

A mixture of 2,2,3,3,4,4,4-heptafluoro-N-[2-(cyanomethyl)phenyl]butanamide (15 g), sodium azide (14.85 g), ammonium chloride (12.22 g) and dimethylformamide (200 mL) was heated in a 130° C. oil bath under a nitrogen atmosphere overnight. The reaction mixture was cooled to room temperature, water (100 mL) was added and the product was extracted with ethylacetate (3×200 mL). The combined extracts were dried over Na2SO4, filtered and concentrated with a rotary evaporator. The brown residue was purified by high pressure liquid chromatography to give a white solid. The solid was triturated with diethyl ether to give 3.2 g of the title compound, m.p. 117°-178° C.

المصدر