vinyl hydrogen sulphate synthesis

Yield:13401-80-4 97.6%

Reaction Conditions:

Stage #1: ethylene glycolwith sodium ethanolate at 5; for 2 h;
Stage #2: with sulfuryl dichloride under 2250.23 - 3000.3 Torr; for 8 h;Flow reactor;Inert atmosphere;Reagent/catalyst;Time;

Steps:

1-8; 1-5 Example 4

S1. Weigh 100kg of ethylene glycol and add it to the synthesis reactor, then add 250kg of sodium ethoxide into the synthesis reactor, then stir for 2h to mix uniformly, and control the temperature in the reactor to 5°C; S2, pass 160kg of sulfuryl chloride into the reaction solution in S1, and the flow rate of sulfuryl chloride is 22mL/min, The inlet pressure is 0.3-0.4MPa, after 2.5 hours of reaction, nitrogen is blown for 1.5 hours, and the reaction is stirred again for 3 hours. After standing for 1 hour, the resulting mixture of vinyl sulfate and metal chloride salt is separated to obtain crude vinyl sulfate. Use anhydrous magnesium sulfate to dehydrate the crude vinyl sulfate, and use dichloroethane to recrystallize the dehydrated crude vinyl sulfate after dehydration. Among them, the weight ratio of dichloroethane to vinyl sulfate is 1.5:1 and finally vacuum drying is carried out to obtain 195.2 kg of high-purity vinyl sulfate. The vacuum degree of vacuum drying is -0.05Mpa and the temperature is 40°C.

References:

CN113563302,2021,A Location in patent:Paragraph 0031-0046