反应 #1730334
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05783647
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A 300-ml four-necked flask equipped with a stirrer, thermometer and dropping funnel was charged with 73.7 g of a 50% hydrogen peroxide aqueous solution. Stirring was started, the flask was kept at a temperature below 20° C. by water cooling, and 51.7 g of 98% conc. sulfuric acid was added dropwise to form a mixed acid. While the flask was cooled at a temperature of 0° to 5° C. with an ice bath, with stirring, 40 ml of a dichloromethane solution containing 42.9 g of 1,1,2,2-tetramethylpropyl alcohol which was previously synthesized according to Journal of the American Chemical Society/89:7/Mar. 29, 1967, was slowly added dropwise. At the end of addition, stirring was continued for a further 2 hours. The reaction solution was washed with pure water until the organic layer became neutral. The organic layer was dried over anhydrous sodium sulfate and distilled of the solvent, yielding 47.4 g of 1,1,2,2-tetramethylpropylhydroperoxide having structural formula (2). A 300-ml four-necked flask equipped with a stirrer was added dropwise to form a mixed acid While the flask was cooled at a temperature of 0° to 5° C. with an ice bath with stirring was previously synthesized 29, 1967, was slowly added dropwise At the end of addition stirring The reaction solution was washed with pure water until the organic layer The organic layer was dried over anhydrous sodium sulfate distilled of the solvent
来源 ID: ord-5a75598cbeef4b5fb672757f832c58bf