Water → 3-Ethoxy-4-hydroxybenzyl 8-methylnonanoate

HRID 1012888

반응식

HRID 1012888 반응식
[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([CH:9]=[CH:10][C:11]=1[OH:12])[CH2:7][OH:8])[CH3:2].[CH3:13][CH:14]([CH3:24])[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][C:21](O)=[O:22].O>CCCCCC>[CH3:13][CH:14]([CH3:24])[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][C:21]([O:8][CH2:7][C:6]1[CH:9]=[CH:10][C:11]([OH:12])=[C:4]([O:3][CH2:1][CH3:2])[CH:5]=1)=[O:22]

참가 물질

5

반응물 3

HCID 962WaterHCID 1114708-Methylnonanoic acidHCID 597767Ethyl vanillyl alcohol

생성물 1

HCID 673169933-Ethoxy-4-hydroxybenzyl 8-methylnonanoate수율 89.1%

시약·촉매·용매 1

HCID 8058Hexane용매

반응 조건

온도
50 °C

실험 절차

3-Ethoxy-4-hydroxybenzyl alcohol (733 mg, 4.35 mmol), 8-methylnonanoic acid (751 mg, 4.35 mmol) and Novozyme 435 (100 mg) were measured and placed in a flask (25 ml). The mixture was stirred with heating in an oil bath at 50° C. for 16 hr without plugging the flask. After stirring with heating for 2 to 3 hr, attachment of water onto the upper wall of the flask was observed. The reaction mixture was allowed to cool to room temperature, hexane (50 ml) was added, and Novozyme 435 and the insoluble material were removed by filtration. Hexane (25 ml) was added to the filtrate, and the mixture was washed with 5% aqueous citric acid solution (25 ml×2) and saturated brine (25 ml) and dried over anhydrous magnesium sulfate. Magnesium sulfate was filtered off, and the filtrate was concentrated under reduced pressure to give 3-ethoxy-4-hydroxybenzyl 8-methylnonanoate (1.25 g, yield 88.8%) as a colorless oil.

후처리

  1. customplaced in a flask
  2. stirringAfter stirring
  3. temperaturewith heating for 2 to 3 hr
  4. temperatureto cool to room temperature
  5. customNovozyme 435 and the insoluble material were removed by filtration
  6. additionHexane (25 ml) was added to the filtrate
  7. washthe mixture was washed with 5% aqueous citric acid solution (25 ml×2) and saturated brine (25 ml)
  8. dry with materialdried over anhydrous magnesium sulfate
  9. filtrationMagnesium sulfate was filtered off
  10. concentrationthe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-663edc46763747b4ab38b2ebb736dff6
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07981460B2

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