HCID 86651899, compound → HCID 58183447, compound

Temperature

60 °C

Next, a four neck flask having a content volume of 200 mL equipped with a thermometer, a distilling head and a stirring device was charged with 137.4 g of water, 42.2 mg of sulfuric acid and 24.2 g (130 mmol) of 3-(2,2-dimethoxyethyloxy)-2-butanol. The mixture was stirred for 11 hours on the conditions of a pressure of 18.0 kPa and a vessel inside temperature of 60° C. while removing water and resulting methanol by distillation. In this regard, the reaction solution was analyzed by gas chromatography to find that a conversion rate of 3-(2,2-dimethoxyethyloxy)-2-butanol was 99.6%. After the vessel inside temperature was lowered down to room temperature, the pH was adjusted to 8.0 by a 10.0 mass % sodium hydroxide aqueous solution, and the reaction solution was extracted three times with 300 g of ethyl acetate. The extracts of three extractions thus obtained were put together and concentrated under reduced pressure, and the concentrate obtained was refined by silica gel chromatography to obtain 9.66 g (72.2 mmol) of 5,6-dimethyl-1,4-dioxane-2-ol in the form of a colorless and transparent oil (purity: 98.8%, yield: 55.5% based on 3-(2,2-dimethoxyethyloxy)-2-butanol).

1. customequipped with a thermometer
2. customwhile removing water
3. customresulting methanol
4. distillationby distillation
5. customwas lowered down to room temperature
6. extractionthe reaction solution was extracted three times with 300 g of ethyl acetate
7. extractionThe extracts of three extractions
8. customthus obtained
9. concentrationconcentrated under reduced pressure
10. customthe concentrate obtained

ORD record

ord-10949f2286de4eb0aec75fbaa9da5078

Source dataset

uspto-grants-2013_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08431722B2