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Efficient mechanical force promoted aliphatic amine preparation method

A fatty amine and mechanical force technology, applied in the preparation of sulfuric acid amide, organic chemistry, etc., to achieve the effect of green reaction conditions, simple product separation, and high safety

Active Publication Date: 2018-08-24
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most amination reactions require toxic organic solvents as reaction solvents, such as benzene, dichloromethane, etc.

Method used

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  • Efficient mechanical force promoted aliphatic amine preparation method
  • Efficient mechanical force promoted aliphatic amine preparation method
  • Efficient mechanical force promoted aliphatic amine preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] In a 50 ml stainless steel mortar and mortar, Rh 2 (esp) 2 (0.001mmol, 0.76mg), 4-ethylbiphenyl (0.3mmol, 54.7mg), 2,2,2-trichloroethylsulfamate (0.2mmol, 45.7mg), iodobenzene diacetate (0.4 mmol, 129 mg), NaHCO 3 (200mg). Put the stainless steel mortar in the ball mill After placing it safely, adjust the speed to 300r / min for 150min and start the machine. After the reaction is finished, lower the temperature to 25°C to 30°C, add dichloromethane to the reaction system, and wash thoroughly three times. The above dichloromethane solution was washed with water three times, the above dichloromethane phase was dried over anhydrous sodium sulfate, filtered and the dichloromethane was concentrated under reduced pressure to obtain a crude product. Use a 100-200-mesh silica gel column for separation, elute with a mixed solvent of petroleum ether / ethyl acetate (20:1), and collect the target product 2,2,2-trichloroethyl (1-([1,1' - biphenyl-4-yl) ethyl) sulfamate], and th...

Embodiment 2

[0044] In a 50 ml stainless steel mortar and mortar, Rh 2 (esp) 2 (0.001mmol, 0.76mg), 4-ethylbiphenyl (0.3mmol, 54.7mg), neopentyl sulfamate (0.2mmol, 33.4mg), iodobenzene diacetate (0.4mmol, 129mg), NaHCO 3 (200mg). Put the stainless steel mortar in the ball mill After placing it safely, adjust the speed to 300r / min for 150min and start the machine. After the reaction is finished, lower the temperature to 25°C to 30°C, add dichloromethane to the reaction system, and wash thoroughly three times. The above dichloromethane solution was washed with water three times, the above dichloromethane phase was dried over anhydrous sodium sulfate, filtered and the dichloromethane was concentrated under reduced pressure to obtain a crude product. Use a 100-200-mesh silica gel column for separation, elute with a mixed solvent of petroleum ether / ethyl acetate (20:1), and collect the target product neopentyl (1-([1,1'-biphenyl-4- base) ethyl) sulfamate], and the organic phase was con...

Embodiment 3

[0048] In a 50 ml stainless steel mortar and mortar, Rh 2 (esp) 2 (0.001mmol, 0.76mg), 4-ethylbiphenyl (0.3mmol, 54.7mg), 4-nitrophenylsulfamate (0.2mmol, 43.6mg), iodobenzene diacetate (0.4mmol, 129mg) , NaHCO 3 (200mg). Put the stainless steel mortar in the ball mill After placing it safely, adjust the speed to 300r / min for 150min and start the machine. After the reaction is finished, lower the temperature to 25°C to 30°C, add dichloromethane to the reaction system, and wash thoroughly three times. The above dichloromethane solution was washed with water three times, the above dichloromethane phase was dried over anhydrous sodium sulfate, filtered and the dichloromethane was concentrated under reduced pressure to obtain a crude product. Use a 100-200 mesh silica gel column for separation, elute with a mixed solvent of petroleum ether / ethyl acetate (25:1), and collect the target product 4-nitrophenyl (1-([1,1'-biphenyl -4-yl) ethyl) sulfamate], and the organic phase ...

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Abstract

The invention discloses an aliphatic amine preparation method. The aliphatic amine preparation method comprises the following steps: taking alkyl, aryl and the like as a substrate 1 and taking a nitrogen source as a substrate 2; adding an additive, an oxidizing agent and a noble metal catalyst which are suitable; and reacting under the effect of mechanical force to obtain aliphatic amine. The provided method is different from traditional organic reaction, addition of any solvents in reaction can be avoided completely, only raw materials are mixed, a target product can be obtained by simple ball-milling through mechanical force, and therefore, the aliphatic amine preparation method has the characteristics of environmental protection, high yield, gentle condition, simplicity and conveniencein operation and the like.

Description

technical field [0001] The invention belongs to the field of fine chemicals and relates to a method for preparing fatty amines. Background technique [0002] The direct amination of C(sp3)-H is an ideal way to construct C-N bonds and synthesize fatty compounds, which are ubiquitous in nature and biologically active molecules, such as alkaloids and alkaloid-like drugs. The development of green synthetic methods without directing groups, under mild conditions, with high efficiency and high selectivity (especially for intermolecular reactions) is a frontier issue for C(sp3)-H amination. After hundreds of years of hard work, organic scientists have proved that transition metals such as Ag, Mn, Fe, Co, Ru, and Rh catalyzed the amination of C(sp3)-H to C(sp3)-H by transition metals such as Ag, Mn, Fe, Co, Ru, and Rh, which is an efficient method for constructing aliphatic amines. The catalytic performance of Rh(II) is the most prominent. However, most amination reactions require...

Claims

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Application Information

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IPC IPC(8): C07C303/34C07C307/02
CPCC07C303/34C07C2601/14C07C307/02
Inventor 钟芳锐卢训博吴钰周张玉龙白玉龙汪雨凡
Owner HUAZHONG UNIV OF SCI & TECH
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