SELENOUREA synthesis
- Product Name:SELENOUREA
- CAS Number:630-10-4
- Molecular formula:CH4N2Se
- Molecular Weight:123.02
Yield:630-10-4 30.1 g
Reaction Conditions:
Stage #1:selenium with sodium tetrahydroborate in ethanol for 0.5 h;Cooling with ice;
Stage #2:carbamimidothioic acid methyl ester with sodium carbonate in ethanol at 20; for 22 h;Reflux;
Steps:
1
Mix 54.4g of methyl chloroacetate and 110ml of dry toluene, cool, and add 31.6g of methyl formate when the temperature drops to 0°C, and then add 28.2g of 97% when the internal temperature drops to -10°C-5°C Sodium methoxide, Reacted for 4h at 5°C, and then reacted for 3h at room temperature, and finally 28.15g yellow oil was obtained. It is the crude product of methyl α-chloroformyl acetate. Take 76g (1mol) of thiourea dissolved in 400ml of absolute ethanol, slowly add 141.90 (1mol) of methyl iodide dropwise, after the dropwise addition, control the temperature at about 40, react until the solution is clear and stop the reaction, cool and stand for crystallization ,filter, Obtained 89.01 g of white crystals, namely methyl isothiourea. In a 1000ml three-necked flask, let nitrogen gas cool, add 7.27g sodium borohydride and 13.63g selenium powder under ice bath, and stir well. Then add 250ml of absolute ethanol dropwise first slowly and then quickly. After the addition, react in an ice bath for 0.5h, then add 170ml of absolute ethanol to dissolve 30.22g of methyl isothiourea solution, then add 14.77g of anhydrous sodium carbonate, reflux for 2h, and react at room temperature for 20h. After the reaction is over, add 34ml of glacial acetic acid to the reaction solution, blow in nitrogen to expel the generated hydrogen selenide and methyl isothiourea gas, add tail gas absorption device, 900ml of 5% lead acetate solution, time for 2-3 hours, and then filter. The filtrate was evaporated under reduced pressure, and stopped when it was evaporated to 80ml-100ml. The filter cake obtained by filtration was the product selenium urea, the crude product was 30.10g.
References:
Maidexin International Co., Ltd.;Zhao Haifeng CN112079794, 2020, A Location in patent:Paragraph 0089; 0097-0099
420-04-2
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$15.00/25g
630-10-4
62 suppliers
$60.00/1g
4338-95-8
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$22.00/1g
630-10-4
62 suppliers
$60.00/1g
