Method for preparing 1-tert butyl-3-(2,6-diisopropyl-4-phenyl cxypheny) thiourea
A technology of phenoxyphenyl and diisopropylaniline, which is applied in the field of preparation of thiourea organic compounds, can solve the problems of many reaction by-products, high raw material prices and high energy consumption, and achieves high total yield and low energy consumption. The effect of energy, simple operation
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Embodiment 1
[0029] (1) Add 4-phenoxy-2,6-diisopropylaniline 4.2g (content 91%, 0.014mol), carbon disulfide 4g (content 99%, 0.052mol), triethylamine 5.3g to the reaction flask (content 99%, 0.052 mol) and toluene 10ml, stirred at 20~25 ℃ for about 14 hours, when the content of 4-phenoxy-2,6-diisopropylaniline in the raw material monitored by HPLC was less than 1%, the reaction ended. A yellow solid precipitated out in the reaction flask and was filtered. The filtrate was reserved for the next application; the filter cake was dried to obtain 6.2 g of solid as triethylamine dithio(4-phenoxy-2,6-diisopropylanilino)formate.
[0030] (2) Put the triethylamine dithio(4-phenoxy-2,6-diisopropylphenylamino)formate solid obtained in the previous step into the reaction flask, add 10ml tert-butylamine and 10ml triethylamine at 20~ Stir at 25°C for about 24 hours, and when the content of triethylamine dithio(4-phenoxy-2,6-diisopropylanilino)formate in the raw material monitored by HPLC is less than 1...
Embodiment 2
[0032] (1) Add 4-phenoxy-2,6-diisopropylaniline 21.0g (content 93%, 0.07mol), carbon disulfide 21.6g (content 99%, 0.28mol) and toluene 100ml in 250ml autoclave, After ammonia replacement, at 20-25°C, 8kg / cm 2 The reaction was continued under pressure with ammonia stirring for about 24 hours. When the content of 4-phenoxy-2,6-diisopropylaniline hydrochloride in the raw material monitored by HPLC was less than 1%, the reaction ended. A yellow ammonium dithio(4-phenoxy-2,6-diisopropylanilino)formate solid precipitated out of the reaction mixture.
[0033] (2) Put the yellow reaction mixture obtained in the previous step into a reaction flask, add 10ml of tert-butylamine and stir at 20-25°C for about 24 hours. The raw material dithio(4-phenoxy-2,6-diisopropyl When the ammonium salt content of anilino)formate is less than 1%, the reaction ends. Excess tert-butylamine and solvent toluene were removed by distillation under reduced pressure, which will be used in the next step; 40m...
Embodiment 3
[0035] (1) Add 23.7g (content 93%, 0.072mol) of 4-phenoxy-2,6-diisopropylaniline hydrochloride to the reaction flask, then add 20ml ammonia (25%) and 25ml water, Add 21.6 g of carbon disulfide (content 99%, 0.28 mol) dropwise under stirring, stir at 20-25°C for about 24 hours, and monitor the content of the raw material 4-phenoxy-2,6-diisopropylaniline hydrochloride by HPLC to be less than 1 %, the reaction ends. A yellow solid precipitated out in the reaction flask and was filtered. The filtrate was reserved for the next application; the filter cake was dried to obtain 25.9 g of solid as dithio(4-phenoxy-2,6-diisopropylanilino)ammonium formate.
[0036](2) Put the solid obtained in the previous step into a reaction flask, add 30 ml of tert-butylamine and stir at 20-25°C for about 24 hours. The raw material dithio(4-phenoxy-2,6-diisopropylbenzene When the amino) ammonium formate content is less than 1%, the reaction ends. Distill under reduced pressure to remove excess tert...
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