Formic Acid → HCID 178466567, Verbindung

HRID 1793274Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1793274
[F:1][C:2]1[C:7]([F:8])=[C:6]([O:9][CH2:10][CH3:11])[CH:5]=[CH:4][C:3]=1[C@H:12]1[CH2:17][CH2:16][C@H:15]([CH2:18][CH2:19][CH:20]2OCCC[O:21]2)[CH2:14][CH2:13]1.C(O)=O>C1(C)C=CC=CC=1>[F:1][C:2]1[C:7]([F:8])=[C:6]([O:9][CH2:10][CH3:11])[CH:5]=[CH:4][C:3]=1[C@H:12]1[CH2:17][CH2:16][C@H:15]([CH2:18][CH2:19][CH:20]=[O:21])[CH2:14][CH2:13]1

Komponenten

4

Edukt 2

HCID 284Formic AcidHCID 178466566HCID 178466566, Verbindung

Produkt 1

HCID 178466567HCID 178466567, VerbindungAusbeute 100 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

The 2-(2-(trans-4-(2,3-difluoro-4-ethoxyphenyl)-cyclohexyl)-ethyl)-1,3-dioxane (19.8 mmol) obtained by the reaction of Step 4 was dissolved in 100 ml of toluene, 87% formic acid (198 mmol) was added, and the solution was heated to reflux for 4 hours. The reaction solution was twice washed with 50 ml of a saturated aqueous solution of sodium hydrogen carbonate, then three times with 50 ml of water, and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, to form crude 3-(trans-4-(2,3-difluoro-4-ethoxyphenyl)-cyclohexyl)-propanal (19.8 mmol).

Aufarbeitung

  1. temperaturethe solution was heated
  2. temperatureto reflux for 4 hours
  3. washThe reaction solution was twice washed with 50 ml of a saturated aqueous solution of sodium hydrogen carbonate
  4. dry with materialthree times with 50 ml of water, and dried over anhydrous magnesium sulfate
  5. distillationThe solvent was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-c5d2a3c98a094bf9b2875bcfff8c573c
Quelldatensatz
uspto-grants-2006_07
Patentnummer
US07081279B2

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