THIOFORMAMIDE synthesis

Yield:115-08-2 75%

Reaction Conditions:

with carbon monoxide;nitrogen at 180 - 200; under 30003 Torr;

Steps:

1 Example 1
In a 2000ml autoclave equipped with a stirrer, inner coil condenser, pressure gauge, and thermometer (design pressure 10MPa),Adding a certain amount of organic base as a catalyst,Cover the kettle lid and make a safety inspection in accordance with regulations.After replacing with nitrogen, 684 g of carbon disulfide, 51 g of liquid nitrogen, and 100.8 g of carbon monoxide were added.After the raw materials are added, the autoclave pressure is increased to 4 MPa by filling with nitrogen.Close the nitrogen gas inlet valve and heat up to 180 ° C within 1 hour to react uniformly.Keep the autoclave pressure at 4 ~ 6MPa, and maintain the temperature at 180 ~ 200 for 6 ~ 8 hours.After the heating is stopped and the inner coil is cooled to below 20 ° C with cooling water,Open the drain pipe to release the pressure to normal pressure, and discharge the generated carbon dioxide gas.The evacuation tube was closed, and the reaction solution was pressurized from the submerged discharge tube to the rectification kettle with nitrogen.
Transfer the above reaction solution to a 2000 mL four-necked flask equipped with a distillation column, an oil bath, and a reflux condenser.The temperature is raised to 50 ° C, and carbon disulfide is recovered. The recovered carbon disulfide can be used to continue the synthesis of thioformamide.The carbon disulfide recovery was completed, and the temperature continued to rise to 120 ° C.Collect about 137.25 g of distillate with a tower top temperature of 103-105 ° C.The yield is 75% in terms of ammonia,After no distillate, continue to warm to 220 ° C,Collect about 27 g of distillate with a tower top temperature of 209 to 211 ° C.The yield was 20% in terms of ammonia.

References:

Meng Xianfeng CN110845378, 2020, A Location in patent:Paragraph 0027-0029

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