Hydrogen Peroxide → HCID 15425388, compound

Temperature

50 °C

After 69 mg (1.18 mmol) of potassium fluoride and 118 mg (1.18 mmol) of potassium hydrogen carbonate were dissolved in 1 ml of methanol, to this solution were added both 2.0 g (17.7 mol) of 30% aqueous hydrogen peroxide and a solution prepared by dissolving, in 1.5 ml of tetrahydrofuran, 165 mg (590 μmol) of dimethyl(5-hydroxy-3,3-dimethylhexyl)(2-pyridyl)silane which had been prepared in the same manner as Example 17. The solution after mixing was continued to be stirred for 22 hours at an inner temperature of 50° C. After cooling to room temperature, 10 ml of water was added to the solution after the reaction, and the mixture was extracted with three portions of 20 ml of diethyl ether. The resulting organic layers were combined together, washed with 20 ml of 15% sodium thiosulfate and dried over sodium sulfate. The solvent was evaporated off under reduced pressure to give crude 2,4,4-trimethyl-2,6-hexanediol. This was purified with a silica gel column using a mixed solvent of hexane/ethyl acetate=1/1 (volume ratio) to give 94 mg of 2,4,4-trimethyl-2,6-hexanediol in the form of colorless oil (Yield: 99%; the purity: >95%).

1. customa solution prepared
2. additionThe solution after mixing
3. temperatureAfter cooling to room temperature
4. customafter the reaction
5. extractionthe mixture was extracted with three portions of 20 ml of diethyl ether
6. washwashed with 20 ml of 15% sodium thiosulfate
7. dry with materialdried over sodium sulfate
8. customThe solvent was evaporated off under reduced pressure
9. customto give crude 2,4,4-trimethyl-2,6-hexanediol
10. customThis was purified with a silica gel column

ORD record

ord-0b5d325a9d114c9987bc3060d554822d

Source dataset

uspto-grants-2003_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06531602B2