Novel isocyanide compound and hydrosilylation reaction catalyst
一种氢化硅烷化、化合物的技术,应用在有机化合物/氢化物/配位配合物催化剂、物理/化学过程催化剂、催化反应等方向,能够解决反应性低、不清楚、处置不容易等问题,达到溶解性好的效果
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[0303] Hereinafter, synthesis examples, examples, and comparative examples are given to describe the present invention in more detail, but the present invention is not limited by the following examples.
[0304] All the solvents used in the preparation of the metal compound were deoxidized and dehydrated by known methods.
[0305] The obtained metal compound was stored at 25°C under a nitrogen atmosphere and used in the reaction.
[0306] The hydrosilylation reaction and solvent purification of olefins were all carried out under an inert gas atmosphere, and solvents used in various reactions were all purified, dried, and deoxygenated by known methods in advance.
[0307] 1 H. 13 C. 19 The F-NMR measurement was performed using JNM-ECA600 and JNM-LA400 manufactured by JEOL Ltd., and the IR measurement was performed using FT / IR-550 manufactured by JASCO Corporation.
[0308] In addition, in the chemical structural formula shown below, hydrogen atoms are omitted according to c...
Synthetic example 1
[0309] [Synthesis example 1] Synthesis of iron pivalate
[0310] The reference J.Cluster.Sci., 2005, 16, 331. was synthesized by the following method.
[0311] 0.86 g (15.4 mmol) of reduced iron and 3.50 g (34.3 mmol) of pivalic acid were added to a 50 mL two-necked eggplant-shaped flask equipped with a reflux tube, and stirred at 160° C. for 12 hours. At this time, the reaction solution changed from colorless and transparent to green. Furthermore, 2.50 g (24.5 mmol) of pivalic acid was added, and it stirred at 160 degreeC for 19 hours. Then, the reaction solution was filtered, combined with the recovered supernatant, and dried at 80°C under reduced pressure. The obtained solid was washed with hexane to obtain a green solid (2.66 g, yield 67%).
[0312] FT-IR (KBr) ν: 2963, 2930, 2868, 1583, 1523, 1485, 1457, 1427, 1379, 1362, 1229, 1031, 938, 900, 790, 608, 576, 457cm -1
Synthetic example 2
[0313] [Synthesis example 2] Synthesis of cobalt pivalate
[0314] With reference to the document Russ.Chem.Bull., 1999, 48, 1751., it was synthesized by the following method.
[0315] Add 1.15 g (6.5 mmol) of cobalt acetate, 1.55 g (15.2 mmol) of pivalic acid, and 0.5 mL (2.5 mmol) of pivalic anhydride into a 50 mL two-necked eggplant-shaped flask with a reflux tube, and stir at 160 ° C. for 1 hour. At this time, the reaction solution changed from light purple to purple. Then, it was dried under reduced pressure at 80° C., and the obtained solid was washed with pentane and diethyl ether, and dried to obtain a purple solid (1.15 g, yield 68%).
[0316] FT-IR (KBr) ν: 2963, 2929, 2868, 1599, 1524, 1485, 1457, 1420, 1379, 1363, 1229, 1032, 938, 900, 792, 613, 585, 460cm -1
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