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ChemicalBook CAS DataBase List Glutarimide
1121-89-7

Glutarimide synthesis

13synthesis methods
To a flask containing 70 gm (0.53 mole) of glutaric acid is added 150 ml (2.2 mole) of 28% aqueous ammonia. The mixture is set for distillation and heated for 7 hr as the temperature of the mixture rises from 90° to 180°C. The temperature is held at 170-180°C for \\ hr or until the evolution of ammonia ceases. The reaction mixture solidifies on cooling and the pro­duct is recrystallized from acetone to afford 37.4 gm (63%), m.p. 145-146°C.
t may be advantageous to preform the ammonium salt of dicarboxylic acids prior to the application of enough heat to form the imide. The preparation of succinimide is a case in point.
Preparation of Glutarimide
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Yield:1121-89-7 98%

Reaction Conditions:

with manganese(II) triflate;4,4'-diamino-2,2'-bipyridyl;dihydrogen peroxide in acetone at 20; for 1 h;Reagent/catalyst;

Steps:

1 Example 1

5.59 mg (0.03 mmol) of 4,4'-diamino-2,2'-bipyridine (Ligand), 5.30 mg (0.015 mmol) of manganese (II) triflate (Mn(OTf) 2),1.5 mL of acetone was added to the reaction tube, and the reaction was stirred at 70 ° C for 10 min.Cool to room temperature and add 49.57 mg (0.5 mmol) of 2-piperidone.Then, 250 μL of 30% by mass of hydrogen peroxide was diluted with 0.5 mL of acetone and then added to the reaction tube through a flow injection pump for 60 minutes.After the addition, saturated sodium sulfite was added to the reaction solution to quench the remaining hydrogen peroxide.Extraction with ethyl acetate gave 1,2-dipiperidone in a yield of 98%.

References:

CN109824465,2019,A Location in patent:Paragraph 0017-0027

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