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Preparation method of bis (triisopropyl cyclopentadienyl) strontium

A technology of triisopropylcyclopentadiene and propylcyclopentadiene is applied in the field of preparation of bis(triisopropylcyclopentadienyl) strontium, and can solve the problems of complicated process operation, difficult purification and high cost problems, to achieve the effect of high metal purity, avoid solvent molecule coordination, and improve yield

Active Publication Date: 2021-10-29
苏州源展材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] It can be seen that the current methods for preparing strontium derivatives generally have problems such as complicated process operation, difficult purification, high cost, and low yield, and the product molecule contains solvent molecule coordination and there are many metal element impurities, resulting in low purity

Method used

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  • Preparation method of bis (triisopropyl cyclopentadienyl) strontium
  • Preparation method of bis (triisopropyl cyclopentadienyl) strontium
  • Preparation method of bis (triisopropyl cyclopentadienyl) strontium

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Experimental program
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Effect test

Embodiment 1

[0032] Under nitrogen protection, add 200 mL of hexamethyldisilazane to a 500 mL reaction flask, start stirring, slowly add 8.96 g of strontium hydride solid powder into the reaction flask through a solid injector, stir to dissolve, and dissolve 48.01 g of 1 , 2,4-triisopropylcyclopentadiene was slowly added dropwise to the reaction flask, refluxed at 130 °C for 24 hours, and the obtained filtrate was evaporated to dryness under reduced pressure to obtain the crude product (off-white waxy solid), which was then sublimated under reduced pressure 40.44 g of bis(triisopropylcyclopentadienyl)strontium (white solid) were obtained, a yield of 86%.

[0033] The product was characterized by NMR, as image 3 As shown, the NMR results are as follows:

[0034] 1 H NMR (500 MHz, C 6 D. 6 ) d (ppm): 5.79 (s, 4H, ring-CH), 3.0(m, 4H, CH), 2.94 (m, 2H, CH), 1.32(m, 36H, CH 3 ).

[0035] The metal purity of the sample was tested by inductively coupled plasma optical emission spectromete...

Embodiment 2

[0037]Under nitrogen protection, add 200 mL of hexamethyldisilazane to a 500 mL reaction flask, start stirring, slowly add 8.96 g of strontium hydride solid powder into the reaction flask through a solid injector, stir to dissolve, and dissolve 48.41 g of 1, 2,4-Triisopropylcyclopentadiene was slowly added dropwise to the reaction flask, refluxed at 130 °C for 24 hours, the obtained filtrate was evaporated to dryness under reduced pressure to obtain the crude product (off-white waxy solid), and then obtained by sublimation under reduced pressure 40.31 g of strontium bis(triisopropylcyclopentadienyl) (white solid), 85% yield.

[0038] The metal purity of the sample was tested by ICP-OES, and the results showed that the metal purity of the sample was 5N.

Embodiment 3

[0040] Under nitrogen protection, add 200 mL of hexamethyldisilazane to a 500 mL reaction flask, start stirring, slowly add 8.96 g of strontium hydride solid powder into the reaction flask through a solid injector, stir to dissolve, and dissolve 48.01 g of 1, 2,4-Triisopropylcyclopentadiene was slowly added dropwise to the reaction flask, refluxed at 130°C for 48 hours, and the obtained filtrate was evaporated to dryness under reduced pressure to obtain the crude product (off-white waxy solid), which was then obtained by sublimation under reduced pressure 40.71 g of strontium bis(triisopropylcyclopentadienyl) (white solid), 87% yield.

[0041] The metal purity of the sample was tested by ICP-OES, and the results showed that the metal purity of the sample was 5N.

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Abstract

The invention discloses a preparation method of bis (triisopropyl cyclopentadienyl) strontium, which comprises the following steps: (1) under a protective atmosphere, dissolving strontium hydride in hexamethyldisilazane to obtain a mixed solution; (2) dropwise adding 1, 2, 4-triisopropyl cyclopentadiene into the mixed solution, and carrying out a reaction under the condition of heating reflux; and (3) after the reaction is finished, collecting a product to obtain the bis (triisopropyl cyclopentadienyl) strontium. The bis (triisopropylcyclopentadienyl) strontium is prepared by a one-pot method, the preparation method is simple, the reaction condition is mild, the energy consumption is low, the safety is high, and the product yield is up to 87%; besides, the problem that a product prepared in the prior art contains solvent molecular coordination and metal impurities is avoided, the metal purity of the product is as high as 5N, and the product can be used as a precursor source material for growing a high-quality SrO film with nano thickness by an atomic layer deposition technology.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of bis(triisopropylcyclopentadienyl)strontium. Background technique [0002] Alkaline earth metal β-diketone compounds are the earliest compounds that can be used as ALD precursors due to their low reactivity and low saturated vapor pressure. Sr( i PR 3 Cp) 2 (where the ligand i PR 3 Cp is 1,2,4-triisopropylcyclopentadienyl) is considered as a very promising strontium source ALD precursor with a melting point of 94 °C and a saturated vapor pressure of 2.5 Torr at 200 °C, Much higher than Sr(tmhd) 2 (0.1Torr, 230°C). Due to the existence of multiple isopropyl groups, the steric hindrance is relatively large, and the ability of the cyclopentadienyl itself to bind to the Sr atom is weak. i PR 3 The bonding strength between the Cp ligand and the Sr metal atom is very weak, and the strontium atom is easily detached from the center of the ligand ...

Claims

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Application Information

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IPC IPC(8): C07F17/00C23C16/40C23C16/455
CPCC07F17/00C23C16/45553C23C16/404
Inventor 陈鹏宇
Owner 苏州源展材料科技有限公司
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