Methanol → 2-Propenoic acid, 3-(4-fluorophenyl)-, methyl ester

HRID 256705

반응식

HRID 256705 반응식
[F:1][C:2]1[CH:12]=[CH:11][C:5]([CH:6]=[CH:7][C:8]([OH:10])=[O:9])=[CH:4][CH:3]=1.[CH3:13]O.S(=O)(=O)(O)O.O>C(OCC)C>[CH3:13][O:9][C:8](=[O:10])[CH:7]=[CH:6][C:5]1[CH:4]=[CH:3][C:2]([F:1])=[CH:12][CH:11]=1

참가 물질

6

반응물 4

HCID 887Methanol2회HCID 962WaterHCID 1118Sulfuric AcidHCID 980703-(4-Fluorophenyl)-2-propenoic acid

생성물 1

HCID 9587502-Propenoic acid, 3-(4-fluorophenyl)-, methyl ester

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A one liter round bottom flask was charged with 50 grams (0.30 moles) of 4-fluorocinnamic acid, 500 milliliters of methanol, and 5.0 grams of concentrated sulfuric acid. This mixture was brought to reflux and kept there for 18 hours. After cooling, one half of the methanol was stripped under vacuum, and the remaining solution was poured into 600 milliliters of water. The precipitated solid was taken into 500 milliliters of diethyl ether and the aqueous phase was discarded. The ether solution was washed three times with 10% aqueous sodium hydroxide and once with water. After drying over magnesium sulfate, the mixture was filtered and stripped under vacuum to give methyl-4-fluorocinnamate as a white crystalline powder. Yield was 40 grams.

후처리

  1. temperatureto reflux
  2. temperatureAfter cooling
  3. washThe ether solution was washed three times with 10% aqueous sodium hydroxide
  4. dry with materialAfter drying over magnesium sulfate
  5. filtrationthe mixture was filtered

출처 및 근거

ORD 기록
ord-cfb318807128447bb7fd55580030b7a4
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05258517

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