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Hydrochloric Acid → HCID 54191570, Verbindung

HRID 728105
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 728105
[Cl-].Cl[CH2:3][C:4](=O)[CH2:5][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[NH2:26][C:27]1[CH:32]=[C:31]([CH3:33])[CH:30]=[CH:29][N:28]=1.[CH2:34]([O:41][C:42]1[CH:43]=[C:44]([CH:47]=[CH:48][C:49]=1[N+:50]([O-:52])=[O:51])[CH:45]=O)[C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1.C(=O)([O-])[O-].[K+].[K+].Cl>C(#N)C.O>[CH2:34]([O:41][C:42]1[CH:43]=[C:44]([CH:45]=[CH:5][C:4]2[N:26]=[C:27]3[CH:32]=[C:31]([CH3:33])[CH:30]=[CH:29][N:28]3[CH:3]=2)[CH:47]=[CH:48][C:49]=1[N+:50]([O-:52])=[O:51])[C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 313Hydrochloric AcidHCID 15332-Amino-4-methylpyridineHCID 11430Potassium Carbonate2×HCID 27736283-Chloro-2-oxopropyl triphenylphosphonium chlorideHCID 121117193-(Benzyloxy)-4-nitrobenzaldehyde

Produkt 1

HCID 54191570
HCID 54191570, Verbindung
Ausbeute 45,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A mixture of (chloroacetonyl)triphenylphosphonium chloride (190.7 g) and 2-amino-4-methylpyridine (158.9 g) in acetonitrile (1.3 l) was stirred under reflux for 5.5 hours. To the reaction mixture were added water (400 ml) and 3-benzyloxy-4-nitrobenzaldehyde (63.0 g) under ice-cooling. The mixture was adjusted to pH 9.5 with potassium carbonate and stirred for 2.5 hours at ambient temperature under keeping the pH 9.5 to 10.0 with 20% aqueous potassium carbonate. The reaction mixture was adjusted to pH 2.0 with conc. hydrochloric acid and the precipitate was collected by filtration. To a mixture of ethyl acetate, tetrahydrofuran and water was added the above obtained precipitate and the resultant mixture was adjusted to pH 7.0 with 20% aqueous potassium carbonate. The separated organic layer was washed with brine and dried over magnesium sulfate. The solvent was removed in vacuo to give 2-[2-(3-benzyloxy-4-nitrophenyl)vinyl]-7-methylimidazo[1,2-a]pyridine (43.14 g).

Aufarbeitung

  1. temperatureunder reflux for 5.5 hours
  2. temperaturecooling
  3. stirringstirred for 2.5 hours at ambient temperature
  4. filtrationthe precipitate was collected by filtration
  5. additionTo a mixture of ethyl acetate, tetrahydrofuran and water
  6. additionwas added the above obtained precipitate
  7. washThe separated organic layer was washed with brine
  8. dry with materialdried over magnesium sulfate
  9. customThe solvent was removed in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-87938e24a82a4465a7dfa21c333e36c3
Quelldatensatz
uspto-grants-1991_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05047411

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