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A hexanuclear drum type organotin carboxylate complex of p-tolyltin and its preparation method and application

A technology of organic tin carboxylate and tolyl tin, which is applied in the direction of tin organic compounds, medical preparations containing active ingredients, compounds of group 4/14 elements of the periodic table, etc., can solve the problem of staying at the structural level, strengthening, The practical application of structural compounds has not been well realized, achieving the effects of low cost, excellent fluorescence performance, and long fluorescence lifetime

Inactive Publication Date: 2019-02-22
JINLIN MEDICAL COLLEGE
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  • Abstract
  • Description
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Problems solved by technology

Usually using organotin substrate [RSn(O)OH] n A hexa-nuclear drum-type organotin carboxylate compound is obtained by reacting with a monobasic organic carboxylic acid at a ratio of 1:1, and many drum-type organotin carboxylate compounds with similar structures have been obtained through this reaction; although there are many existing drum-type structures, However, the practical application of compounds with this structure has not been well realized. More research is still focused on the conversion between this structure and other structures, still at the structural level, and few have been discovered and used for catalytic activity. , electrical activity, and photosensitivity test experiments; therefore, it is particularly important to strengthen the research on the properties of hexa-core drum-type organotin carboxylate compounds in various application directions

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  • A hexanuclear drum type organotin carboxylate complex of p-tolyltin and its preparation method and application
  • A hexanuclear drum type organotin carboxylate complex of p-tolyltin and its preparation method and application
  • A hexanuclear drum type organotin carboxylate complex of p-tolyltin and its preparation method and application

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preparation example Construction

[0033] The present invention also provides a preparation method of a hexanuclear drum-type organotin carboxylate complex of p-tolyltin, comprising: sequentially adding 1,8-naphthalene diimide propionic acid and di For p-tolyl tin oxide, add benzene solution, stir and reflux for at least 8 hours, naturally cool to room temperature, filter, evaporate the filtrate naturally to obtain a white powder, recrystallize, and place it to obtain a colorless crystal, which is the hexa-nuclear drum-type organotin Carboxylate complexes.

[0034] In another embodiment, the ratio of 1,8-naphthalene diimide propionic acid to the amount of di-p-tolyltin oxide is 1-1.5:0.8-1.2, and the stirring and reflux reaction time is 8-12 hours , the stirring and reflux reaction temperature is 80-90°C, the initial mass-volume concentration of di-p-tolyltin oxide is 1 / 45mmol / mL~1 / 65mmol / mL, toluene solution is used for recrystallization, and the initial mass-volume concentration is 8-9g / L, 8 Recrystallize th...

Embodiment 1

[0040] Preparation of organotin carboxylate complexes: Add 1 mmol of 1,8-naphthalimide propionic acid and 1 mmol of di-p-tolyltin oxide to the reaction vessel in sequence, add 60 ml of benzene solution to dissolve, and stir at 80°C Reflux for 8 hours, naturally cool to room temperature and filter, evaporate the filtrate naturally to obtain a white solid powder, use 50ml of toluene for recrystallization, and place it for 6 days to obtain colorless crystals, the yield is 85%, and the melting point is >300°C;

[0041] The structural formula of the resulting product is:

[0042]

[0043] Carry out elemental analysis, theoretically calculated value (C 132 h 102 N 6 o 30 sn 6 ·C 7 h 8 ): C, 54.62; N, 2.75; H, 3.63; test value: C, 54.59; N, 2.78; H, 3.60;

[0044] Such as figure 1 Shown, infrared spectroscopic analysis: IR (KBr, cm -1 ): 1701v (O=C); 1585v as (COO); 1438v s(COO); 630v (Sn-C); 492ν (Sn-O);

[0045] Such as figure 2 Shown, proton nuclear magnetic reson...

Embodiment 2

[0048] Preparation of organotin carboxylate complex: Add 1mmol of 1,8-naphthalimide propionic acid and 0.8mmol of di-p-tolyltin oxide to the reaction vessel in sequence, add 36ml of benzene solution to dissolve, and dissolve at 90°C Stir and reflux for 9 hours, naturally cool to room temperature and filter, evaporate the filtrate naturally to obtain a white solid powder, use 50ml of toluene for recrystallization, leave it for 8 days to obtain colorless crystals, the yield is 83%, melting point: >300°C.

[0049] The structural formula of the resulting product is:

[0050]

[0051] Carry out elemental analysis, theoretically calculated value (C 132 h 102 N 6 o 30 sn 6 ·C 7 h 8 ): C, 54.62; N, 2.75; H, 3.63; test value: C, 54.59; N, 2.78; H, 3.60;

[0052] Such as figure 1 Shown, infrared spectroscopic analysis: IR (KBr, cm -1 ): 1701v (O=C); 1585v as (COO); 1438v s (COO); 630v (Sn-C); 492ν (Sn-O);

[0053] Such as figure 2 Shown, proton nuclear magnetic resonanc...

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Abstract

The invention discloses a p-tolyltin hexanuclear drum-type organotin carboxylate complex, which is a compound of the following structural formula (1). The invention also discloses a preparation method and application of a hexanuclear drum-type organotin carboxylate complex of p-tolyltin.

Description

technical field [0001] The invention relates to the field of organotin carboxylate complexes, in particular to a hexanuclear drum-type organotin carboxylate complex of p-tolyltin and its preparation method and application. Background technique [0002] E. Frankland first synthesized the organotin compound Et in 1894 2 SnI 2 , This move opened the prelude to the development of organotin chemistry research. In 1972, Crowe proposed and studied the anticancer activity of organotin complexes in detail, which made organotin chemistry develop rapidly. It has been found that organotin compounds have higher antitumor activity than cisplatin compounds, and have attracted widespread attention because of their diverse structures, various types, and wide applications. So far, the research on organotin compounds has involved many fields such as organometallic chemistry, structural chemistry, coordination chemistry, biochemistry and pharmacology, which makes organotin chemistry one of th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/22A61K31/555C09K11/06A61P35/00
CPCC07F7/2224C09K11/06C09K2211/188
Inventor 肖箫徐坤崔桂花
Owner JINLIN MEDICAL COLLEGE
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