Acetic Anhydride → HCID 22759330, Verbindung

HRID 1704374Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1704374
[C:1]([CH:4]([CH2:14][CH2:15][CH2:16][CH:17]([OH:27])[CH2:18][O:19][C:20]1[CH:25]=[CH:24][C:23]([F:26])=[CH:22][CH:21]=1)[CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][C:11]([OH:13])=[O:12])(=[O:3])[CH3:2].[C:28](OC(=O)C)(=[O:30])[CH3:29]>CCOCC>[C:1]([CH:4]([CH2:14][CH2:15][CH2:16][CH:17]([O:27][C:28](=[O:30])[CH3:29])[CH2:18][O:19][C:20]1[CH:25]=[CH:24][C:23]([F:26])=[CH:22][CH:21]=1)[CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][C:11]([OH:13])=[O:12])(=[O:3])[CH3:2]

Komponenten

4

Versuchsvorschrift

A mixture of 8-acetyl-12-hydroxy-13-(4-fluorophenoxy)tridecanoic acid (9.5 g., 0.025 mole) and acetic anhydride (6.1 g., 0.06 mole) is heated at 60° for 18 hours. The mixture is then cooled and dissolved in 80 ml. of ether. The solution is extracted with an ice-cold solution of 8 g. of sodium hydroxide in 150 ml. of water. The basic solution is separated and acidified with concentrated hydrochloric acid. The oily acid that separates is taken up in ether, washed with water and dried over sodium sulfate. The ether is evaporated to leave the crude product as a viscous yellow oil.

Aufarbeitung

  1. temperatureis heated at 60° for 18 hours
  2. temperatureThe mixture is then cooled
  3. dissolutiondissolved in 80 ml
  4. extractionThe solution is extracted with an ice-cold solution of 8 g
  5. customThe basic solution is separated
  6. washwashed with water
  7. dry with materialdried over sodium sulfate
  8. customThe ether is evaporated

Quellen und Nachweise

ORD-Eintrag
ord-b435a123f6b54907b3d706d427a2ceee
Quelldatensatz
uspto-grants-1978_11
Patentnummer
US04126629

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