تفاعل #2487412

معادلة التفاعل

water

sodium diethyldithiocarbamate trihydrate

4-vinylbenzyl chloride

→

Diethyl-Dithiocarbamic Acid 4-Vinyl-Phenyl Ester

المذيبات

ethanol

ethanol

ظروف التفاعل

المعالجة

1. 1
   أخرىequipped with a stirrer
2. 2
   استخلاصextracting with diethyl ether
3. 3
   غسيلThe ether phase was washed three times with water
4. 4
   تجفيفdried over sodium sulphate
5. 5
   أخرىbefore finally removing the diethyl ether
6. 6
   أخرىby evaporation
7. 7
   أخرىThe residue was recrystallised three times from methanol
8. 8
   أخرىgiving a yield of 2.6 grams (83%)

الإجراء التجريبي

A solution of sodium diethyldithiocarbamate trihydrate (3.5 g, 1.55×10−2 mol) in 20 mL of ethanol was added to a flask equipped with a stirrer, dropping funnel and a reflux condenser. To this solution was added a solution of 4-vinylbenzyl chloride (3.0 g, 1.96×10−2 mol) and ethanol (5 mL), dropwise, over a period of 0.5 h at a temperature of 0° C. The resultant solution was stirred at room temperature for 24 h before pouring into a large volume of water and extracting with diethyl ether. The ether phase was washed three times with water, dried over sodium sulphate, before finally removing the diethyl ether by evaporation. The residue was recrystallised three times from methanol, giving a yield of 2.6 grams (83%). 1H NMR (CDCl3) δ7.36 (s, 4H, C6H4), 6.70 (dd, J=11.6 and 17.5 Hz, 1H, CH═CH2), 5.73 (d, J=17.5 Hz, 1H, CH═CH2), 5.24 (d, J=11.5 Hz, 1H, CH═CH2), 4.54 (s, 2H, CH2S), 4.04 (q, J=7.3 Hz, 2H, NCH2), 3.73 (q, J=6.6 Hz, 2H NCH2), 1.19 (t, J=ca.7.0 Hz, 6H CH2CH3).

المصدر