反应 #2487412

反应方程式

water

sodium diethyldithiocarbamate trihydrate

4-vinylbenzyl chloride

→

Diethyl-Dithiocarbamic Acid 4-Vinyl-Phenyl Ester

溶剂

ethanol

ethanol

反应条件

后处理

1. 1
   其他equipped with a stirrer
2. 2
   萃取extracting with diethyl ether
3. 3
   洗涤The ether phase was washed three times with water
4. 4
   干燥dried over sodium sulphate
5. 5
   其他before finally removing the diethyl ether
6. 6
   其他by evaporation
7. 7
   其他The residue was recrystallised three times from methanol
8. 8
   其他giving a yield of 2.6 grams (83%)

实验过程

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).

来源