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Sodium borohydride → HCID 57570973, Verbindung

HRID 1695305
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1695305
C([O:3][C:4]([C:6]1[CH:11]=[C:10]([O:12][CH2:13][CH2:14][CH2:15][NH:16][C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])[CH:9]=[C:8]([C:24](OCC)=[O:25])[N:7]=1)=O)C.[BH4-].[Na+].[Cl-].[Ca+2].[Cl-].[H][H]>C(O)C>[C:20]([O:19][C:17]([NH:16][CH2:15][CH2:14][CH2:13][O:12][C:10]1[CH:9]=[C:8]([CH2:24][OH:25])[N:7]=[C:6]([CH2:4][OH:3])[CH:11]=1)=[O:18])([CH3:23])([CH3:21])[CH3:22]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 4311764Sodium borohydrideHCID 5284359Calcium ChlorideHCID 67145385HCID 67145385, VerbindungHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 57570973HCID 57570973, VerbindungAusbeute 67,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702
Ethanol
Lösungsmittel

Versuchsvorschrift

To a solution of 4-(3-tert-butoxycarbonylamino-propoxy)-pyridine-2,6-dicarboxylic acid diethyl ester (150 mg) in absolute ethanol (5 mL) was added sodium borohydride (43 mg) and calcium chloride (128 mg). After stirring for 4 h, hydrogen evolution ceased, and reaction was quenched with water. Solvent was evaporated under reduced pressure. The residue was then washed into separatory funnel using dichloromethane and water. The layers were separated, and the aqueous layer was extracted three times with dichloromethane. The combined organic solutions were dried over magnesium sulphate, and concentrated in vacuo to give 4-(3-tert-butoxycarbonylamino-propoxy)-2,6-bis-(hydroxymethyl)pyridine (80 mg):

Aufarbeitung

  1. customreaction
  2. customwas quenched with water
  3. customSolvent was evaporated under reduced pressure
  4. washThe residue was then washed into separatory funnel
  5. customThe layers were separated
  6. extractionthe aqueous layer was extracted three times with dichloromethane
  7. dry with materialThe combined organic solutions were dried over magnesium sulphate
  8. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-9f31a6c0ebfe4bed80ccf0f989f387d4
Quelldatensatz
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08163736B2

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