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Cyclohexanimine synthesis

15synthesis methods
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Yield:22554-30-9 93.3%

Reaction Conditions:

with ammonia in methanol; for 3 h;Sealed tube;Cooling with ice;Reagent/catalyst;

Steps:

1-5; 1

General procedure: In a cylindrical container (capacity 500 ml, outer diameter 80 mm, made of glass), 100 g of cyclohexanone, 10 g of molecular sieve 3A (manufactured by Shinwa Kako Co., Ltd.) and a stirrer were placed and sealed with a rubber stopper. Next, two SUS pipes with a diameter of 6 mm were passed through the rubber stopper, one was connected to the exhaust pipe and inserted up to 1 cm from the inner surface of the rubber stopper, and the other was connected to the ammonia supply pipe and inserted until it was 1 cm above the stirrer. .. Then, ammonia was supplied at 50 g / hour and stirred at room temperature. At this time, the room temperature was 30 ° C. The amount of the liquid in the container was measured 3 hours after the supply of ammonia, and 0.5 μL of the liquid in the container was collected and analyzed by gas chromatography. The cyclohexanone conversion rate 3 hours after the supply of ammonia was 63.2%. The cyclohexaneimine selectivity was 15.8% and the cyclohexaneimine yield was 10.0%.

References:

JP2020/189809,2020,A Location in patent:Paragraph 0025-0030