تفاعل #1990024

معادلة التفاعل

hydrogen chloride

sodium

1H-1,2,4-triazole

1H-1,2,4-triazole

NaOH

2-cyano-2-(2,4-dichlorophenyl) decyl bromide

→

hydrochloric salt

المردود 28.2%

1-[2-Cyano-2-(2,4-dichlorophenyl)decyl]-1,2,4-triazole

المردود 28.2%

المذيبات

ether

water

DMSO

ظروف التفاعل

المعالجة

1. 1
   أخرىprepared by the usual route)
2. 2
   درجة الحرارةThe mixture is then cooled
3. 3
   استخلاصThe organic material which separates is extracted 2×100 ml of ether
4. 4
   غسيلthe extract is washed 2×50 ml of water
5. 5
   تجفيفdried over anhydrous magnesium sulfate
6. 6
   تركيزconcentrated
7. 7
   أخرىto give 24.0 g (82.5%) of the crude product
8. 8
   أخرىThe solid which precipitates
9. 9
   أخرىis separated by filtration

الإجراء التجريبي

To 7.0 g (0.07697 mole) of the sodium salt of 1H-1,2,4-triazole, generated from 5.3 g; (0.07697 mole) of 1H-1,2,4-triazole and 3.1 g (0.759 mole) of NaOH, in 50 ml of DMSO, is added 30.0 g (0.0767 mole) of 2-cyano-2-(2,4-dichlorophenyl) decyl bromide (prepared by the usual route); and the reaction is stirred at 130° for 20 hours. The mixture is then cooled and mixed with 200 ml of water. The organic material which separates is extracted 2×100 ml of ether, and the extract is washed 2×50 ml of water, dried over anhydrous magnesium sulfate and concentrated to give 24.0 g (82.5%) of the crude product. This material is dissolved in ether, and it is treated with hydrogen chloride gas until it is acidic to litmus. The solid which precipitates is separated by filtration to give 9.0 g (28.2%) of the hydrochloric salt, mp 125°-31°. To 6.7 g (0.0161 mole) of the hydrochloride salt in 200 ml of water is stirred. The organic soluble material is extracted 2×200 ml of ether, and the extract is washed 2×50 ml of water, dried over anhydrous magnesium sulfate, and concentrated to give 4.9 g (80.2%) of the oil product.

المصدر