Hydrochloric Acid → Ethyl 2-benzylacrylate

HRID 1109415노트

반응식

HRID 1109415 반응식
[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

참가 물질

9

반응물 5

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

생성물 1

HCID 11084648Ethyl 2-benzylacrylate

시약·촉매·용매 3

HCID 962Water용매HCID 8028Tetrahydrofuran용매2회HCID 8857Ethyl Acetate용매

실험 절차

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 separted, 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.

후처리

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

출처 및 근거

ORD 기록
ord-09c351fddedf4acca6714cfaafb99991
출처 데이터셋
uspto-grants-1994_06
특허 번호
US05319082

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