Water → HCID 22759220, Verbindung

HRID 460857Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 460857
[Na].[F:2][C:3]([F:12])([F:11])[C:4]1[CH:5]=[C:6]([OH:10])[CH:7]=[CH:8][CH:9]=1.[C:13]([CH:16]([CH2:28][CH2:29][CH2:30][CH:31]1[O:33][CH2:32]1)[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][C:23]([O:25][CH2:26][CH3:27])=[O:24])(=[O:15])[CH3:14].O>C(O)C.CCOCC>[C:13]([CH:16]([CH2:28][CH2:29][CH2:30][CH:31]([OH:33])[CH2:32][O:10][C:6]1[CH:7]=[CH:8][CH:9]=[C:4]([C:3]([F:11])([F:12])[F:2])[CH:5]=1)[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][C:23]([O:25][CH2:26][CH3:27])=[O:24])(=[O:15])[CH3:14]

Komponenten

7

Versuchsvorschrift

Sodium (1.15 g., 0.05 mole) is dissolved in ethanol (60 ml.). 3-Trifluoromethylphenol (14.6 g., 0.09 mole) is added and then ethyl 8-acetyl-12,13-epoxytridecanoate (13.0 g., 0.0435 mole). The resulting solution is heated under reflux for 1.5 hour. It is then cooled and poured into 300 ml. of water. The oily product is taken up in ether, washed with 100 ml. of 5% sodium hydroxide solution, water and brine and dried over sodium sulfate. The ether is evaporated in vacuo leaving 17.4 g. of the title compound as a yellow oil. It is used in the next step without purification.

Aufarbeitung

  1. temperatureThe resulting solution is heated
  2. temperatureunder reflux for 1.5 hour
  3. temperatureIt is then cooled
  4. additionpoured into 300 ml
  5. washwashed with 100 ml
  6. dry with materialof 5% sodium hydroxide solution, water and brine and dried over sodium sulfate
  7. customThe ether is evaporated in vacuo
  8. customleaving 17.4 g

Quellen und Nachweise

ORD-Eintrag
ord-e667d5947a244450ad0d3127302f43e4
Quelldatensatz
uspto-grants-1977_12
Patentnummer
US04061643

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