تفاعل #363320

معادلة التفاعل

4-(aminosulphonyl)phenylhydrazine

(E)-1,1,1-trifluoro-4-(4-methylphenyl)-3-butene-2-one

water

→

1-(4-aminosulphonylphenyl)-4,5-dihydro-5-(4-methylphenyl)-3-trifluoromethyl-1H-pyrazole

المردود 45.0%

المذيبات

acetic acid

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةIt is cooled
2. 2
   استخلاصextracted with AcOEt
3. 3
   غسيلThe organic solution is washed with water
4. 4
   تجفيفdried over anhydrous sodium sulphate
5. 5
   أخرىevaporated to dryness under vacuum
6. 6
   أخرىThe crude product thus obtained
7. 7
   أخرىis crystallised from EtOH-petrol ether

الإجراء التجريبي

A solution of 4-(aminosulphonyl)phenylhydrazine chlorohydrate (0.82 g, 3.69 mmoles) and (E)-1,1,1-trifluoro-4-(4-methylphenyl)-3-butene-2-one (0.79 g, 3.69 mmoles) in 15 ml of acetic acid is refluxed for 3 hours under a nitrogen atmosphere. It is cooled, poured over water and extracted with AcOEt. The organic solution is washed with water, dried over anhydrous sodium sulphate and evaporated to dryness under vacuum. The crude product thus obtained is crystallised from EtOH-petrol ether to give 1-(4-aminosulphonylphenyl)-4,5-dihydro-5-(4-methylphenyl)-3-trifluoromethyl-1H-pyrazole (0.65 g, yield: 45%).

المصدر