ChemicalBook CAS DataBase List tert-Butyl hydroperoxide

tert-Butyl hydroperoxide synthesis

13synthesis methods

Product Name:tert-Butyl hydroperoxide
CAS Number:75-91-2
Molecular formula:C4H10O2
Molecular Weight:90.12

TBHP is produced by the liquid-phase reaction of isobutane and molecular oxygen or by mixing equimolar amounts of t-butyl alcohol and 30–50% hydrogen peroxide. TBHP can also be prepared from t-butyl alcohol and 30% hydrogen peroxide in the presence of sulfuric acid or by oxidation of tert-butylmagnesium chloride. The manufacturing process of TBHP is in a closed system.

75-64-9
457 suppliers
$10.00/10g

75-91-2
216 suppliers
$26.00/100g

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

75-28-5 Synthesis