tert-Butyl hydroperoxide synthesis
- Product Name:tert-Butyl hydroperoxide
- CAS Number:75-91-2
- Molecular formula:C4H10O2
- Molecular Weight:90.12
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75-91-2
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Yield:75-91-2 98.8%
Reaction Conditions:
Stage #1: tert-butylaminewith sodium hydrogen sulfate;1,2-dibutoxyethane;lead(IV) tetraacetate;oxalic acid at 26; for 2.33333 h;
Stage #2: with cobalt(II) nitrate at 45; for 4 h;Temperature;
Steps:
3 A method for synthesizing a t-butyl hydroperoxide pharmaceutical intermediate comprises the following steps:
A: 2 mol of 2-methyl-2-propylamine was added to the reaction vessel.900ml mass fraction is 17% sodium sulfate solution,Control the stirring speed to 160 rpm and control the solution temperature to 26 ° C.Add 6 mol of lead tetraacetate,6mol ethylene glycol dibutyl ether solution,4 mol of 21% oxalic acid solution was added in 4 portions over 50 min.Continue to react for 90 minutes;B: Then add 4 mol of cobalt nitrate powder, raise the temperature of the solution to 45 ° C, continue the reaction for 4 h, reduce the temperature to 10°C, the solution was layered, washed with a mass fraction of 16% potassium nitrate solution for 30 min, added with a mass fraction of 37% ethyl bromide solution for 60 min, and recrystallized in a mass fraction of 55% 1-pentene solution.Dehydrated with anhydrous sodium sulfate dehydrating agent,The finished t-butyl hydroperoxide was 177.84 g, and the yield was 98.8%.
References:
CN108239008,2018,A Location in patent:Paragraph 0012; 0017; 0018; 0021-0026
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75-91-2
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75-91-2
192 suppliers
$26.00/100g