Five-core tin (II) compound and preparation method and application thereof

A compound, the technology of trimethylsilylbenzene, applied in the field of pentanuclear tin compounds and its preparation, can solve the problems of high cost of rare earth metals and complicated synthesis process, and achieve low synthesis cost, high sample purity and novel compound structure Effect

Active Publication Date: 2019-04-23
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the cost of rare earth metals used in catalyst synthesis is high, and the synthesis process is relatively complicated

Method used

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  • Five-core tin (II) compound and preparation method and application thereof
  • Five-core tin (II) compound and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Preparation of pentanuclear tin (II) compound a: Add 0.50 g (2.92 mmol) lithium trimethylsilylphenyl (base) amide to a weighed reaction flask under nitrogen protection, add 30 ml of ether, and place in an acetone bath Dimethylaminonitrile (0.24ml, 2.92mmol) was added under the conditions, reacted overnight, and SnCl was added under the conditions of the acetone bath. 2 (0.69g, 3.65mmol), slowly warmed up to room temperature, and reacted overnight. Stand still, filter, the filtrate is concentrated under vacuum, and crystallize at room temperature, and a colorless crystal is precipitated to obtain 0.256 g of pentanuclear tin (II) compound a, with a yield of 24.4%.

[0014] Melting point: 138-141°C

[0015] Elemental analysis: theoretical value C, 33.04; H, 3.74; N, 11.56%; found value C, 33.01; H, 3.72; N, 11.65.

[0016] NMR: 1 H NMR (CDCl 3 ):δ1.69(THF),2.57(s,12H,N(CH 3 ) 2 ),3.21(s,12H,N(CH 3 ) 2 ), 3.76(THF), 4.10(s,2H,NH),7.02-7.38(m,20H,Ph). 13 C NMR (CDCl...

Embodiment 2

[0018] Step 1, the preparation of pentanuclear tin (II) compound a is the same as in Example 1.

[0019] Step 2, the addition reaction of aniline and N,N'-diisopropylcarbodiimide: Weigh 0.015g (0.01mmol) of compound a into a 30mL Schlenk bottle filled with nitrogen, add N,N' - Diisopropylcarbodiimide 0.31 mL (2.00 mmol) and aniline 0.18 mL (2.00 mmol). Reacted at 25°C for 1.0h, hydrolyzed with 0.5mL of water, extracted three times with 30mL of dichloromethane (3×10mL), anhydrous Na 2 SO 4 Dry and filter. The filtrate was sucked dry, and the product was crystallized and purified with n-hexane to obtain the product guanidine with a yield of 80.4%.

Embodiment 3

[0021] Step 1, the preparation of pentanuclear tin (II) compound a is the same as in Example 1.

[0022] Step 2, the addition reaction of aniline and N,N'-diisopropylcarbodiimide: Weigh 0.015g (0.01mmol) of compound a into a 30mL Schlenk bottle filled with nitrogen, add N,N' - Diisopropylcarbodiimide 0.31 mL (2.00 mmol) and aniline 0.18 mL (2.00 mmol). Reacted at 25°C for 2.0h, hydrolyzed with 0.5mL of water, extracted three times with 30mL of dichloromethane (3×10mL), anhydrous Na 2 SO 4 Dry and filter. The filtrate was pumped dry, and the product was crystallized and purified with n-hexane to obtain the product guanidine with a yield of 84.6%.

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Abstract

The invention provides a five-core tin (II) compound and a preparation method and an application thereof. A synthetic process of the compound comprises the following steps: under the protection of a nitrogen gas, adding trimethyl silicon-based benzene (phenyl) lithium amide to a reaction vessel, adding ethyl ether for dissolving, in a condition of an acetone bath, adding dimethylaminonitrile, reacting overnight, and adding SnCl2 in the condition of the acetone bath, slowly warming to a room temperature, reacting overnight, stewing, filtering, concentrating filtrate in vacuum, crystalizing in the room temperature, and separating out a colorless crystal, to obtain the five-core tin (II) compound, wherein a mole ratio of the trimethyl silicon-based benzene (phenyl) lithium amide, the dimethylaminonitrile and the SnCl2 is 1:1:1-1.25. The compound can be used as a catalyst, and used for catalyzing a reaction of generating guanidine by aniline and N,N'-diisopropyl carbodiimide addition, andhas better application prospect.

Description

technical field [0001] The invention relates to polynuclear metal compounds, in particular to a pentanuclear tin (II) compound constructed on the basis of divalent tin ions and guanidinium ligands, and a preparation method and application thereof. Background technique [0002] have CN 3 As an organic base, the guanidine compound can catalyze Michael addition reaction, Henry reaction, addition and esterification reaction of phosphite and unsaturated carbonyl compound, and play an important role in the fields of pharmaceuticals, organometallics, coordination chemistry and organic synthesis. play an increasingly important role. [0003] Symmetrical substituted guanidines with functional groups have important applications in the biological and pharmaceutical industries, and their synthesis is often obtained by the catalytic addition of amines and carbodiimides. The catalyst used is semi-sandwich type, bridging amidino, β-diimine or similar β-ketoamine and other ligand-supporte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/22B01J31/22C07C277/08C07C279/18
CPCB01J31/1805B01J2231/4277B01J2531/0205B01J2531/0213B01J2531/42C07C277/08C07F7/2284C07C279/18
Inventor 周梅素王迎迎郭则灵
Owner SHANXI UNIV
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