Boron trifluoride → HCID 21954468, compound

In a 50 mL four-necked flask, 0.5 g of α,α,β-trimethyl-β-methacryloyloxymethyl-β-propiolactone was put, and dissolved in 10 g of ethyl acetate, and a stirrer, a thermometer and a Dimroth cooling tube were connected thereto. Further, 5 mol % of diethyl ether complex of boron trifluoride was added thereto based on the substrate, and 5 mg of p-methoxyphenol was added thereto, and while solution temperature was kept at 30° C., the resulting mixture was stirred. After the mixture was stirred for 2 hours, the resulting reaction mixture was washed with a 10% sodium carbonate aqueous solution and saturated brine, and dried over magnesium sulfate. After separation by filtration, the solvent was distilled off using an evaporator. A quantitative isomerization reaction to crude α,α,β-trimethyl-β-methacryloyloxy-γ-butyrolactone represented by formula (9) was confirmed. FIG. 2 shows an NMR measurement chart.

1. temperaturea stirrer, a thermometer and a Dimroth cooling tube
2. additionwas added
3. customwas kept at 30° C.
4. stirringAfter the mixture was stirred for 2 hours
5. customthe resulting reaction mixture
6. washwas washed with a 10% sodium carbonate aqueous solution and saturated brine
7. dry with materialdried over magnesium sulfate
8. customAfter separation
9. filtrationby filtration
10. distillationthe solvent was distilled off
11. customan evaporator
12. customA quantitative isomerization reaction to crude α,α,β-trimethyl-β-methacryloyloxy-γ-butyrolactone

ORD record

ord-47a302d6d84b4fa98475e536215d3f4c

Source dataset

uspto-grants-2016_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09346775B2