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Boron trifluoride → 3-Methyl-5-oxooxolan-3-yl 2-methylprop-2-enoate

HRID 526801
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HRID 526801 반응식
[C:1]([O:6][CH2:7][C:8]1(C)[O:12][C:10](=[O:11])[CH2:9]1)(=[O:5])[C:2]([CH3:4])=[CH2:3].B(F)(F)F.[CH3:18]OC1C=CC(O)=CC=1>C(OCC)(=O)C>[C:1]([O:6][C:7]1([CH3:18])[CH2:8][O:12][C:10](=[O:11])[CH2:9]1)(=[O:5])[C:2]([CH3:4])=[CH2:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6356Boron trifluorideHCID 90154-MethoxyphenolHCID 72550462HCID 72550462, 화합물

생성물 1

HCID 220262473-Methyl-5-oxooxolan-3-yl 2-methylprop-2-enoate

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

In a 50 mL four-necked flask, 0.5 g of β-methacryloyloxymethyl-β-methyl-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. Then, 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. Consequently, 0.42 g of crude β-methacryloyloxy-β-methyl-γ-butyrolactone represented by formula (8) was obtained, and a quantitative isomerization reaction was confirmed by HPLC and NMR.

후처리

  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. customwas obtained
  13. customa quantitative isomerization reaction

출처 및 근거

ORD 기록
ord-baa47cfefb7b4b8a9295fd0df56290a3
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09346775B2

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