Dicyclopropane methylamine synthesis
- Product Name:Dicyclopropane methylamine
- CAS Number:13375-29-6
- Molecular formula:C7H13N
- Molecular Weight:111.18
1453-52-7
13375-29-6
General procedure for the synthesis of (dicyclopropylmethyl)amine from dicyclopropylketone oxime: In a 500 mL autoclave, 100 g of dicyclopropylketone oxime, 6 g of Ruanne nickel, 350 mL of water, and 10 g of sodium hydroxide were added in sequence. After replacing the air in the kettle with nitrogen three times, hydrogen was introduced. The hydrogen pressure of the reaction system was controlled to be 2 MPa, and the temperature was maintained at 70-80 °C for 4 hours. Upon completion of the reaction, the hydrogen pressure was released, the reaction mixture was cooled with continuous stirring, and the nickel catalyst in Nguyen was removed by filtration. The aqueous phase was extracted three times with 200 mL of dichloromethane, and the organic phases were combined and purified by distillation. Fractions from 100-110 °C were collected at a pressure of 100 mmHg to obtain the target product dicyclopropylmethylamine. About 81 g of product was finally obtained in 85.8% yield.
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Yield: 85.8%
Reaction Conditions:
with nickel;sodium hydroxide in water at 70 - 80; under 15001.5 Torr; for 4 h;Inert atmosphere;Autoclave;Reagent/catalyst;Temperature;
Steps:
4 Preparation of bicyclopropylmethylamine by catalytic hydrogenation
In a 500 ml autoclave, 100 g of bicyclopropyl ketoxime, 6 g of Raney nickel, 350 ml of water and 10 g of sodium hydroxide were added.Then nitrogen was replaced three times, and hydrogen was introduced. Control reactor hydrogen pressure of 2Mpa, the temperature is 70-80 ,After 4 hours, the reaction was completed. Discharge, cooling, stirring, suction, remove Rennes nickel.And then extracted with dichloromethane 200ml three times, combined methylene chloride solution, distillation.Collect 100mmHg, 100-110 fractions, that is, product bicyclopropyl methylamine. A total of about 81 g of product was obtained in a yield of 85.8%.
References:
Chengdu Syns Medical Technology, Co.,LTD;Han, WeiHua;Huang, Song CN104672093, 2016, B Location in patent:Paragraph 0027-0028
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13375-29-6
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$9.00/100mg