반응 #2487412

반응 방정식

water

sodium diethyldithiocarbamate trihydrate

4-vinylbenzyl chloride

→

Diethyl-Dithiocarbamic Acid 4-Vinyl-Phenyl Ester

용매

ethanol

ethanol

반응 조건

후처리

1. 1
   기타equipped with a stirrer
2. 2
   추출extracting with diethyl ether
3. 3
   세척The ether phase was washed three times with water
4. 4
   건조dried over sodium sulphate
5. 5
   기타before finally removing the diethyl ether
6. 6
   기타by evaporation
7. 7
   기타The residue was recrystallised three times from methanol
8. 8
   기타giving a yield of 2.6 grams (83%)

실험 절차

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).

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