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

HRID 526801
ノート
印刷プレビュー

反応式

HRID 526801 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6356Boron trifluorideHCID 90154-MethoxyphenolHCID 72550462HCID 72550462、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-baa47cfefb7b4b8a9295fd0df56290a3
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09346775B2

反応ノート

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