Sodium Hydroxide → HCID 57285652, Verbindung

HRID 648660Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 648660
[N:1]1([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[CH:13]([CH:17]([C:29]([NH2:31])=[O:30])[C:18]2[CH:28]=[CH:27][C:21]([C:22](OCC)=[O:23])=[CH:20][CH:19]=2)[CH2:14][CH2:15][CH3:16])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[Na+]>O1CCCC1>[N:1]1([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[CH:13]([CH:17]([C:29]([NH2:31])=[O:30])[C:18]2[CH:19]=[CH:20][C:21]([CH2:22][OH:23])=[CH:27][CH:28]=2)[CH2:14][CH2:15][CH3:16])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 20145118HCID 20145118, VerbindungHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 57285652HCID 57285652, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

A solution of 5.0 gm (11.83 m mol) of ethyl 4-[(1-(2-piperidino-phenyl)-1-butyl)-aminocarbonylmethyl]-benzoate in 75 ml of absolute tetrahydrofuran was added dropwise, at an internal temperature of 0° C., to a stirred suspension of 0.68 gm (17.95 m mol) of lithium aluminium hydride in 25 ml of absolute tetrahydrofuran. The mixture was stirred for 20 hours at ambient temperature and then cooled to 0° C., and 4N sodium hydroxide solution was slowly added dropwise thereto until a filterable precipitate formed. The mixture was filtered, and the precipitate was decocted several times with ether. The combined organic solutions were concentrated by evaporation in vacuo. The evaporation residue was distributed between water and ether. The ether phase was dried, filtered, and concentrated by evaporation in vacuo. The evaporation residue was purified by column chromatography on silica gel [toluene/acetone (5:1)].

Aufarbeitung

  1. temperaturecooled to 0° C.
  2. customuntil a filterable precipitate formed
  3. filtrationThe mixture was filtered
  4. concentrationThe combined organic solutions were concentrated by evaporation in vacuo
  5. dry with materialThe ether phase was dried
  6. filtrationfiltered
  7. concentrationconcentrated by evaporation in vacuo
  8. customThe evaporation residue was purified by column chromatography on silica gel [toluene/acetone (5:1)]

Quellen und Nachweise

ORD-Eintrag
ord-d4e62fc588d44899a207ba65363bfa9e
Quelldatensatz
uspto-grants-1988_04
Patentnummer
US04735959

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