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40167-20-2

N-(METHYLTHIO)PHTHALIMIDE 97 synthesis

4synthesis methods
-

Yield:40167-20-2 96.22%

Reaction Conditions:

with pyridine in ethanol at 10 - 40; for 36 h;Temperature;Reagent/catalyst;Solvent;

Steps:

1-4 Example 4

In a 2000ml four-necked flask equipped with a mechanical stirrer, water bath, dropping funnel, reflux condenser and thermometer, add 80g (0.49mol) N-hydroxyphthalimide, 8g pyridine and 800g anhydrous ethanol, 70g (1.45mol) methyl mercaptan was added dropwise with stirring. With the dropping of methyl mercaptan, the system slightly exothermed. Control the dropping rate so that the system temperature does not exceed 10°C. After the addition was completed, the reaction was stirred at 40°C for 36 hours. After the heat preservation is over, the reaction solution is transferred to a rotary evaporator to distill off excess methyl mercaptan and ethanol. Add 200ml of new methanol to the bottom of the bottle and heat until it is transparent. Crystallize at 0°C for 5 hours. Pour out and filter, wash the filter cake with water until it is neutral, and dry to obtain 91 g of white needle-like crystalline powder, which is N-methylthio phthalimide. The melting range is 177.0-178.3, and the content measured by gas chromatography external standard method is 98.89%. The molar yield based on N-hydroxyphthalimide was 96.22%.

References:

CN111393353,2020,A Location in patent:Paragraph 0008; 0010-0017

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