ChemicalBook CAS DataBase List 3-Methylbutanenitrile

3-Methylbutanenitrile synthesis

11synthesis methods

Product Name:3-Methylbutanenitrile
CAS Number:625-28-5
Molecular formula:C5H9N
Molecular Weight:83.13

590-86-3 Synthesis

590-86-3
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$10.00/5g

625-28-5
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$64.20/5g

Yield:625-28-5 88%

Reaction Conditions:

Stage #1:isovaleraldehyde with hydroxylamine hydrochloride;sodium hydroxide in water at 70;
Stage #2: with copper diacetate;hydrazine in acetonitrile at 90; for 0.5 h;Temperature;

Steps:

1.S1; 1.S2 Example 1
S1, hydroxylammonium hydrochloride (121 g, 1.74 mol) was dissolved in water (200 mL)After stirring and clarifying, pump A was used at a rate of 3.66 g/min.Sodium hydroxide (69.7 g, 1.74 mol) was dissolved in water (200 mL) with pump B at 3.07 g/minThe speed of the pump and the pump B simultaneously into the first 15.9 meters long coil,The coil is immersed in an ice water bath, after the two materials are thoroughly mixed and cooled,Isovaleraldehyde (100 g, 1.16 mol) was pumped into the second 51-meter-long coil with a pump C at a rate of 1.14 g/min, and the coil was immersed in a 70 ° C oil bath in an ice water bath. Export sampling HPLC, product purity of 97% to 99%,The effluent system enters a 1L liquid separation column for liquid separation operation to obtain 105.5g of product.Yield 90%;S2, after 100 g of hydrazine is uniformly dissolved in 100 mL of acetonitrile, it is labeled as solution A,4.5 g of copper acetate was dissolved in 400 mL of acetonitrile, and after stirring, it was solution B.The 3-stage CSTR was connected in series in a 90 ° C oil bath with a CSTR volume of 50 mL per stage.Pump A was pumped at a rate of 1.35 g/min to the first stage CSTR (continuously stirred reactor system) and pump B was pumped with 2.64 g/mL to the first stage CSTR.The third-stage CSTR has a total retention time of 0.5 h, and the third-stage CSTR samples the GC.The conversion of the raw materials was complete, the purity of the system was 98%. After the pumping was completed, the system was directly rectified, and the fraction of 128-132 ° C was collected to obtain 72 g of isovaleronitrile with a yield of 88%.

References:

Liaoning Kailaiying Pharmaceutical And Chemical Co., Ltd.;Hong Hao;Lu Jiangping;Zhang Enxuan;Liu Zhiqing;Zhang Tao;Zhao Qian CN108530319, 2018, A Location in patent:Paragraph 0035; 0036; 0037; 0041; 0042; 0044; 0045; 0049

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107-85-7 Synthesis