Dimethylformamide → 8-Vinyl-1,4-dioxaspiro[4,5]decane

温度

3 °C

233.0 g of the compound (21) and 800 mL of DMF were added to a reactor under nitrogen atmosphere, and stirred at 3° C. under cooling with ice. 92.9 g of potassium t-butoxide (t-BuOK) was added thereto by dividing into 10 portions at a temperature range of from 3 to 10° C. over 2 hours, followed by further stirring at 0° C. for 3 hours. After confirming that the reaction had been completed by GC analysis, the reaction mixture was poured into and mixed with a mixture of 1,500 mL of heptane and 1,500 mL of water at 0° C. The mixture was separated into an organic layer and an aqueous layer by standing still, so as to attain extraction to the organic layer. The resulting organic layer was fractionated and washed with water, followed by drying over anhydrous magnesium sulfate. The resulting organic layer was purified by silica gel column chromatography using heptane as eluent, and the solvent was removed by distillation under reduced pressure. The resulting residue was distilled under reduced pressure to obtain 103.3 g of 8-vinyl-1,4-dioxaspiro[4,5]decane (22) as a colorless transparent liquid.

1. temperatureunder cooling with ice
2. stirringby further stirring at 0° C. for 3 hours
3. additionthe reaction mixture was poured into and
4. customThe mixture was separated into an organic layer
5. extractionextraction to the organic layer
6. washwashed with water
7. dry with materialby drying over anhydrous magnesium sulfate
8. customThe resulting organic layer was purified by silica gel column chromatography
9. customthe solvent was removed by distillation under reduced pressure
10. distillationThe resulting residue was distilled under reduced pressure

ORDレコード

ord-69fd013b738e4342b40e8a3fd3a1a083

出典データセット

uspto-grants-2010_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07695777B2