午夜插插,噜噜噜影院,啪啪伊人网,欧美熟夫,景甜吻戏视频,男人强操性感蕾丝美女视频在线网站,日本美女跳舞视频

Welcome to chemicalbook!
Chinese English Japanese Germany Korea
400-158-6606
Try our best to find the right business for you.
Do not miss inquiry messages Please log in to view all inquiry messages.

Welcome back!

ChemicalBook CAS DataBase List Triethylsilane
617-86-7

Triethylsilane synthesis

13synthesis methods
A synthetic method of triethylsilane comprises the following steps: reacting sodium hydride with trimethyl borate to prepare trimethoxy sodium borohydride; adding triethylchlorosilane to trimethoxy sodium monohydroborate to react to obtain triethylsilane.
To a 500ml reaction flask, 20g (0.5mol) of 60% sodium hydride and 80g of anhydrous tetrahydrofuran were added. Stirring and cooling to 0-10 ℃ under the protection of nitrogen, the mixture was then maintained under nitrogen protection, stirred, and the liquid temperature at 0-10 ℃, and dropwise added 57.2g (0.55mol) of trimethyl borate. After the dropwise addition, the temperature was kept at 0-10 ℃ and stirred for 1 hour.Maintaining the nitrogen protection, stirring and liquid temperature of the reaction liquid at 0-10 ℃, and then dropwise adding 67.7g (0.45mol) of triethylchlorosilane. After the dropwise addition, continuously keep the temperature at 0-10 ℃ and stir for 1 hour. The reaction solution was then filtered at room temperature. Rectifying the filtrate at normal pressure and collecting fractions with the boiling range of 109-110 ℃ as triethylsilane to obtain 46.1g of triethylsilane, which yields 88.2%. 45-64 ℃: a mixed solution of trimethyl borate and tetrahydrofuran; 64-109 ℃:a mixture of tetrahydrofuran and a small triethylsilane.
-

Yield:617-86-7 88%

Reaction Conditions:

with sodium tetrahydroborate in acetonitrile at 20; for 0.25 h;Inert atmosphere;

Steps:

2.2-3 Synthesis of example 3

After replacing the interior of a 7 mL test tube equipped with a stirring bar with nitrogen gas,Under nitrogen flow,In this test tube,0.5 mL of acetonitrile as a reaction solvent,As a reducing agent, sodium borohydride (NaBH 4, ReagentPlus (registered trademark), manufactured by Sigma-Aldrich Japan Co.,Purity 99%) 37.8 mg (1.0 mmol)To prepare a suspension.83.9 μL (0.5 mmol) of triethylchlorosilane (Et 3 SiCl) was added dropwise to this suspension using a microsyringe,The reaction was allowed to proceed for 15 minutes while stirring at room temperature.After the reaction, 18.6 mg (0.1 mmol) of ferrocene was added as a reference substance for calculating the NMR yield.A part of the obtained mixed solution was dissolved in heavy chloroform (CDCl 3)As a result of 1 H NMR measurement, it was found that triethylsilane (Et 3 SiH 4) was produced with an NMR yield of 88% (reference material: ferrocene).

References:

JP2017/160160,2017,A Location in patent:Paragraph 0039; 0041

Triethylsilane Related Search: