Molecular Formula | C6H10O3 |
Molar Mass | 130.1418 |
Physical and Chemical Properties | Chemical Properties The refractive index of the product is 1.4290(25 ℃). |
Use | Use of pharmaceutical intermediates. |
Using tert-butanol as raw material, first oxidize with hydrogen peroxide to obtain tert-butyl hydrogen peroxide, then esterify with acetic anhydride to obtain tert-butyl peroxyacetate, and finally condensed with tetrahydrofuran. 1. Oxidation Add tert-butanol to the reaction tank, add hydrogen peroxide at 35 ℃ under stirring, then raise the temperature to 50 ℃, add 70% sulfuric acid dropwise, add it at about 0.5h, and react at 55-60 ℃ for 5h. Let it stand and delaminate, separate the lower water layer, add anhydrous sodium sulfate to the upper oil layer, dry it, leave it overnight, and filter to obtain tert-butyl hydrogen peroxide 2. Esterification Add acetic anhydride, sodium acetate and benzene to the reaction tank in turn, and add tert-butyl hydrogen peroxide dropwise at 20±5 ℃. After adding, react at 15-20 ℃ for 45min. Then 8% ammonium sulfate solution is added, stirred for 5min, left to stand and stratified, separated into water layer, washed once with 8% ammonium sulfate solution, adjusted to pH7-8 with 10% sodium carbonate solution, separated into alkali liquid layer, dried with anhydrous sodium sulfate in oil layer, filtered, distilled into filtrate to recover benzene, distilled under reduced pressure, collected 43-54 ℃/2.0-2.27kPa fraction, and obtained tert-butyl peroxyacetate. 3. Condensation Add tetrahydrofuran and cuprous bromide to the reaction tank, pass nitrogen for 5min, slowly add tert-butyl peroxyacetate dropwise, add about 0.5h, turn on an ultraviolet lamp, and react at 45-50 ℃ for 26h. Then the tetrahydrofuran was recovered and the fraction above 70 ℃/2.93kPa was collected by distillation under reduced pressure to obtain 2-acetoxytetrahydrofuran. Raw material consumption quota: glacial acetic acid (95%)1638 kg/t, ammonia water (20%)950 kg/t.