StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Acetic Acid → Ethyl 2-(4-(benzyloxy)-2-methoxybenzylidene)-3-oxobutanoate

HRID 2387849
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2387849
[CH2:1]([O:8][C:9]1[CH:16]=[CH:15][C:12]([CH:13]=O)=[C:11]([O:17][CH3:18])[CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:19]([O:25][CH2:26][CH3:27])(=[O:24])[CH2:20][C:21]([CH3:23])=[O:22].C(O)(=O)C.N1CCCCC1>C1(C)C=CC=CC=1>[CH2:1]([O:8][C:9]1[CH:16]=[CH:15][C:12]([CH:13]=[C:20]([C:21](=[O:22])[CH3:23])[C:19]([O:25][CH2:26][CH3:27])=[O:24])=[C:11]([O:17][CH3:18])[CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 176Acetic Acid2×HCID 8082Piperidine2×HCID 8868Ethyl AcetoacetateHCID 42939904-Benzyloxy-2-methoxybenzaldehyde

Produkt 1

HCID 68413560Ethyl 2-(4-(benzyloxy)-2-methoxybenzylidene)-3-oxobutanoate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140
Toluene
Lösungsmittel
2×

Versuchsvorschrift

A solution of 4-(benzyloxy)-2-methoxybenzaldehyde (28.3 g), ethyl acetoacetate (18 ml), acetic acid (1.74 ml) and piperidine (0.56 ml) in toluene (400 ml) was heated under reflux for 48 h. A solution of acetic acid (1.74 ml) and piperidine (0.56 ml) in toluene (10 ml) was added and the solution heated under reflux for a further 48 h. The solvent was evaporated under reduced pressure and the residue partitioned between EtOAc and brine. The organics were separated, washed with aq NaHCO3 soln, 1M HCl, brine, dried and evaporated under reduced pressure to give the subtitle compound, 40 g (used crude in next step).

Aufarbeitung

  1. temperatureunder reflux for 48 h
  2. temperaturethe solution heated
  3. temperatureunder reflux for a further 48 h
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue partitioned between EtOAc and brine
  6. customThe organics were separated
  7. washwashed with aq NaHCO3 soln
  8. dry with material1M HCl, brine, dried
  9. customevaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-065d6b5f09fe4b41bcc5fd86bcbd7d5a
Quelldatensatz
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08268990B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion