HCID 11299135, 화합물 → Ethyl 2-phenylbenzoate

HRID 650324노트

반응식

HRID 650324 반응식
[C:1]1([C:7]2[CH:12]=[CH:11][CH2:10][CH2:9][C:8]=2[C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1>C(O)(=O)C.O.[Pd]>[C:1]1([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

5

반응물 1

HCID 11299135HCID 11299135, 화합물

생성물 1

HCID 9920952Ethyl 2-phenylbenzoate수율 80%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 176Acetic Acid용매HCID 962Water용매

실험 절차

A mixture of ethyl 2-phenylcyclohexa-1,3-dienecarboxylate(90 mg, 0.395 mmol) and 5%Pd/C(50 mg) in acetic acid(1.5 ml) and water(1.5 ml) was refluxed for 2 hr. The reaction mixture was filtrated and the solvent was evaporated under reduced pressure. Toluene was added to the residue and it was dried over MgSO4. After removal of the solvent, the residue was purified by column chromatography on silica gel with n-hexane-AcOEt to afford 71 mg of ethyl 2-phenylbenzoate(y=80.0%) as a pale yellow oil. 1H-NMR(ppm, 300 MHz, CDCl3) δ 7.82(1H, dd, J=1.4 and 7.7 Hz), 7.10-7.60(8H), 4.08(2H, d, J=7.0 Hz), 0.98(3H, t, J=7.0 Hz)

후처리

  1. temperaturewas refluxed for 2 hr
  2. filtrationThe reaction mixture was filtrated
  3. customthe solvent was evaporated under reduced pressure
  4. additionToluene was added to the residue and it
  5. dry with materialwas dried over MgSO4
  6. customAfter removal of the solvent
  7. customthe residue was purified by column chromatography on silica gel with n-hexane-AcOEt

출처 및 근거

ORD 기록
ord-1cf6d04affc548699bae26d6fc291772
출처 데이터셋
uspto-grants-2001_08
특허 번호
US06271418B1

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