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4-Propylbenzoic acid → Methyl 4-propylbenzoate

HRID 1506334
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HRID 1506334 반응식
[CH2:1]([C:4]1[CH:12]=[CH:11][C:7]([C:8]([OH:10])=[O:9])=[CH:6][CH:5]=1)[CH2:2][CH3:3].[CH3:13][Si](C=[N+]=[N-])(C)C>CO.ClCCl>[CH2:1]([C:4]1[CH:12]=[CH:11][C:7]([C:8]([O:10][CH3:13])=[O:9])=[CH:6][CH:5]=1)[CH2:2][CH3:3]
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참가 물질

5

반응물 2

HCID 1376014-Propylbenzoic acidHCID 167693Trimethylsilyldiazomethane

생성물 1

HCID 12861010Methyl 4-propylbenzoate수율 97%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

To a 0° C. solution of 4-propylbenzoic acid (2 g, 12.18 mmol) in methanol (3.00 mL) and dichloromethane (10 mL) was added trimethylsilyldiazomethane (7.92 mL, 15.83 mmol), dropwise over a period of 5 min. Towards the end of the addition, the reaction mixture was pale yellow. The reaction was stirred at 0° C. for 30 min. and the excess diazo reagent was quenched by the slow addition of acetic acid at 0° C. (˜1.5 mL). The colorless solution was concentrated and partitioned between ether (20 mL) and sat. aq. sodium bicarbonate (10 mL). The ether layer was washed with brine (10 mL), dried over sodium sulfate and concentrated to yield methyl 4-propylbenzoate (2.1 g, 11.78 mmol, 97% yield) as a liquid. 1H NMR (400 MHz, CDCl3) δ ppm 7.95 (d, J=8.28 Hz, 2H) 7.24 (d, J=8.53 Hz, 2H) 3.90 (s, 3H) 2.61-2.67 (m, 2H) 1.59-1.71 (m, 1H) 0.94 (t, J=7.40 Hz, 1H).

후처리

  1. additionTowards the end of the addition
  2. customthe excess diazo reagent was quenched by the slow addition of acetic acid at 0° C. (˜1.5 mL)
  3. concentrationThe colorless solution was concentrated
  4. custompartitioned between ether (20 mL) and sat. aq. sodium bicarbonate (10 mL)
  5. washThe ether layer was washed with brine (10 mL)
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-3cdd155ac82741eca505d5f92c98c7c5
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09216972B2

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