Trinuclear iron containing carbonyl cationic compounds as well as preparation method and application thereof

A technology of compound and carbonyl cation, which is applied in the field of trinuclear iron carbonyl cation compounds and their preparation, to achieve the effect of being beneficial to storage and simple preparation process steps

Active Publication Date: 2018-09-28
JIAXING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the development of CORMs compounds with water solubility, good biocompatibility and controllable CO release is of great significance and is also very challenging.

Method used

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  • Trinuclear iron containing carbonyl cationic compounds as well as preparation method and application thereof
  • Trinuclear iron containing carbonyl cationic compounds as well as preparation method and application thereof
  • Trinuclear iron containing carbonyl cationic compounds as well as preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Example 1: [Fe 3 (μ-SCH 2 CH 3 ) 6 (CO) 6 ] + [I 3 ] - Compound preparation

[0041] (1)[Fe(CO) 4 I 2 ] Compound preparation. Under argon protection and ice bath conditions, containing 10mL of Fe(CO) 5 Add the dry THF solution (30mL) that is dissolved with 19.5g iodine dropwise in the dry THF solution (70mL), reaction solution produces gas immediately, and its solution color changes from bright yellow to dark red, stops reaction after infrared spectrum detects no raw material peak . The reaction liquid was concentrated to 10 mL, and 100 mL of petroleum ether was added, and a large amount of black solid product was precipitated immediately, with a yield of 30.5 g (yield 94.1%). FTIR(DCM,ν CO / cm -1 ): 2134, 2111, 2084.

[0042] (2)[Fe 2 (μ-SCH 2 R) 3 (CO) 5 I] Preparation of compounds. Under the protection of argon, put Fe(CO) into the 250mL Schleck reaction flask 4 I 2 (4 g, 9.48 mmol) was added to 50 mL of freshly distilled THF. Under stirring in...

example 2

[0044] Example 2: [Fe 3 (μ-SCH 2 CH 3 ) 6 (CO) 6 ] + [FeBr 4 ] - Compound preparation

[0045] (1)[Fe(CO) 4 Br 2 ] Compound preparation. Under argon protection and ice bath conditions, containing 10mL of Fe(CO) 5 The dry THF solution (70mL) that dissolves 4mL bromine (76.5mmol) is dripped into the dry THF solution (30mL) of 4mL bromine (76.5mmol). The reaction was stopped after the peak. The reaction solution was concentrated to 10 mL, and 100 mL of petroleum ether was added, and a large amount of black solid product was precipitated immediately, with a yield of 22.3 g (yield 90%). FTIR(DCM,ν CO / cm -1 ): 2134, 2090, 2070.

[0046] (2)[Fe 2 (μ-SCH 2 R) 3 (CO) 5 Br] compound preparation. Under the protection of argon, add 3.123g Fe(CO) into the 250mL Schleck reaction flask 4 Br 2 (9.48mmol), 50mL of freshly steamed THF, under ice bath and stirring, add 720μL of ethanethiol (9.48mmol), and then use a normal pressure dropping funnel to dissolve 30mL of new t...

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Abstract

The invention discloses trinuclear iron containing carbonyl cationic compounds as well as a preparation method and application thereof. A structural general formula of the compound is as shown in thedescription, wherein R is methyl or ethyl, Y is [I3] or [FeBr4] negative ions, two iron nucleuses at terminals are of positive bivalency, and the middle iron nucleus is of positive trivalency. The preparation process is simple in steps, and ionic compounds containing trinuclear mixed valence iron can be obtained. The prepared trinuclear iron containing carbonyl cationic compounds have appropriatestability and water solubility, are favorable for storage and transportation, are capable of controlling CO release, and can serve as catalysts to be applied during electrocatalytic reduction of proton hydrogen desorption.

Description

technical field [0001] The invention relates to the technical fields of energy, catalysis and medicinal chemistry. More specifically, the present invention relates to trinuclear iron-containing carbonyl cation compounds and their preparation methods, as well as their use as carbon monoxide releasing molecules in controlled release of carbon monoxide, and as cheap hydrogen production catalysts in electrocatalytic proton reduction hydrogen desorption. Background technique [0002] Iron carbonyl compounds are typical and common compounds among transition metal carbonyl compounds, and have a wide range of applications in organic synthesis, industrial catalysis, energy, medicine and other fields. For example, mononuclear and dinuclear iron carbonyl compounds, because of their chemical structures highly similar to those of the metal catalytic active centers of [Fe]-hydrogenase and [FeFe]-hydrogenase, have been used as biomimetic catalysts for biomimetic catalytic hydrogen producti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/02B01J31/22C25B11/06
CPCB01J31/226B01J2231/62B01J2531/842C07F15/02C25B11/075
Inventor 肖志音刘小明蒋冉郭朱明
Owner JIAXING UNIV
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