Methylparaben → Methyl 4-(allyloxy)benzoate

HRID 257830

反応式

HRID 257830 の反応式
[OH:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:18](Br)[CH:19]=[CH2:20]>CC(C)=O>[CH2:20]([O:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:10][CH:11]=1)[CH:19]=[CH2:18]

参加物

5

反応物 3

HCID 7456MethylparabenHCID 7841Allyl bromideHCID 11430Potassium Carbonate

生成物 1

HCID 4645407Methyl 4-(allyloxy)benzoate収率 86%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A 2 L flask was equipped with a mechanical stirrer, a reflux condenser and a stopper, then charged with 50.05 g (0.329 mol) of methyl 4-hydroxybenzoate, 960 mL of acetone, 22.50 g (1.625 mol) of anhydrous potassium carbonate, 80.5 mL (112.6 g, 0.932 mol) of allyl bromide and the mixture was stirred and refluxed for 14 hours. The mixture was cooled to room temperature, filtered and concentrated to an oil. The residual oil was purified by distillation (97° C. @ 0.03 mm Hg) to afford 53.52 g (86%) of the title compound.

後処理

  1. customA 2 L flask was equipped with a mechanical stirrer, a reflux condenser
  2. temperaturerefluxed for 14 hours
  3. filtrationfiltered
  4. concentrationconcentrated to an oil
  5. distillationThe residual oil was purified by distillation (97° C. @ 0.03 mm Hg)

出典と根拠

ORDレコード
ord-964d5f58841d4a3c80a26641e99c4a23
出典データセット
uspto-grants-1993_11
特許番号
US05264439

関連ノート

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