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Boron trifluoride → 2-Propenoic acid, 2-methyl-, tetrahydro-5-oxo-3-furanyl ester

HRID 526804
ノート
印刷プレビュー

反応式

HRID 526804 の反応式
[C:1]([O:6][CH2:7][CH:8]1[O:12][C:10](=[O:11])[CH2:9]1)(=[O:5])[C:2]([CH3:4])=[CH2:3].B(F)(F)F>C1(C)C=CC=CC=1>[C:1]([O:6][CH:7]1[CH2:8][O:12][C:10](=[O:11])[CH2:9]1)(=[O:5])[C:2]([CH3:4])=[CH2:3]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6356Boron trifluorideHCID 57796750beta-Methacryloyloxymethyl-beta-propiolactone

生成物 1

HCID 114010112-Propenoic acid, 2-methyl-, tetrahydro-5-oxo-3-furanyl ester収率 55%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
30 °C

実験手順

In a 20 mL Schlenk flask, 2.0 g of crude β-methacryloyloxymethyl-β-propiolactone was put, and dissolved in 8.0 g of toluene. Further, 54 μL of diethyl ether complex of boron trifluoride was added thereto, and the resulting mixture was warmed to 30° C. and stirred. After the mixture was stirred for 2 hours, the resulting reaction mixture was washed with a 10% sodium hydrogen carbonate aqueous solution and saturated brine, and dried over magnesium sulfate. After separation by filtration, the solvent was distilled off using an evaporator to give 1.1 g of crude β-methacryloyloxy-γ-butyrolactone represented by formula (10). FIG. 3 shows an NMR measurement chart.

後処理

  1. stirringAfter the mixture was stirred for 2 hours
  2. customthe resulting reaction mixture
  3. washwas washed with a 10% sodium hydrogen carbonate aqueous solution and saturated brine
  4. dry with materialdried over magnesium sulfate
  5. customAfter separation
  6. filtrationby filtration
  7. distillationthe solvent was distilled off
  8. customan evaporator

出典と根拠

ORDレコード
ord-64390162edaf468e91ddd3c8a63dff37
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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