Hydrochloric Acid → Ethyl 2-benzylacrylate

HRID 893148ノート

反応式

HRID 893148 の反応式
[Cl-].[Li+].C(OP([CH:11]([CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[C:12]([O:14][CH2:15][CH3:16])=[O:13])(OCC)=O)C.[CH2:24]1CCN2C(=NCCC2)CC1.C=O.Cl>C1COCC1.C(OCC)(=O)C.O>[CH2:17]([C:11](=[CH2:24])[C:12]([O:14][CH2:15][CH3:16])=[O:13])[C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1

参加物

9

反応物 5

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 27008935085-32-6HCID 433294Lithium Chloride

生成物 1

HCID 11084648Ethyl 2-benzylacrylate

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

1.0 g of lithium chloride was suspended in 20 ml of THF, and 5 g of ethyl 2-diethylphosphono-3-phenylpropionate was dropwise added thereto. The mixture was stirred at room temperature for seven minutes. Then, 3.6 ml of DBU was added thereto and further 11 minutes later, a suspension of 0.72 g of paraformaldehyde in THF (20 ml) was added thereto at 0° C. The mixture was stirred at room temperature overnight. Then, the mixture was neutralized with 1N hydrochloric acid, and water and ethyl acetate were added thereto. The organic layer was separated, and washed with a saturated sodium chloride aqueous solution and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (n-hexane/ethyl acetate=20/1) to obtain 2.4 g of ethyl 2-benzylacrylate as colorless oily substance.

後処理

  1. additionwas added
  2. customat 0° C
  3. stirringThe mixture was stirred at room temperature overnight
  4. additionwere added
  5. customThe organic layer was separated
  6. washwashed with a saturated sodium chloride aqueous solution
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationThe solvent was distilled off under reduced pressure
  9. customthe residue was purified by silica gel column chromatography (n-hexane/ethyl acetate=20/1)

出典と根拠

ORDレコード
ord-fcaff02ef7d646b0868c7fb52702e971
出典データセット
uspto-grants-1992_06
特許番号
US05122523

反応ノート

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