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Sodium borohydride → Benzyl carbamate

HRID 38457
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 38457
[CH2:1]([O:8][C:9](=[O:21])[NH:10]C1CC2C(=O)C(CSC2)C1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[BH4-].[Na+]>C(O)C>[CH2:1]([O:8][C:9](=[O:21])[NH2:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 4311764Sodium borohydride3×HCID 67075315(9-Oxo-3-thia-bicyclo[3.3.1]non-7-yl)-carbamic acid benzyl ester

Produkt 1

HCID 12136Benzyl carbamateAusbeute 40,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

To a solution of (9-oxo-3-thia-bicyclo[3.3.1]non-7-yl)-carbamic acid benzyl ester (16, 4.2 g, 13.7 mmol) in ethanol (172 ml) was added sodium borohydride (0.78 g, 20.6 mmol) portionwise at room temperature. The solution was stirred for 1 hour before addition of sodium borohydride (0.2 g, 5 mmol). The reaction mixture was stirred for 2 days, a further portion of sodium borohydride (0.340 g, 9 mmol) was added, and stirring was continued for 4 hours. The mixture was then concentrated under reduced pressure and cold water was added to the residue as well as dichloromethane. After a extraction of the aqueous phase with dichlormethane, the combined organic layer was dried over anhydrous sodium sulphate, filtered and concentrated under reduced pressure. The crude product was purified by silica gel chromatography (cyclohexane:ethyl acetate 40:60) to yield 9-hydroxy-3-thia-bicyclo[3.3.1]non-7-yl)-carbamic acid benzyl ester as a white solid (0.84 g).

Aufarbeitung

  1. stirringstirring
  2. waitwas continued for 4 hours
  3. concentrationThe mixture was then concentrated under reduced pressure and cold water
  4. additionwas added to the residue as well as dichloromethane
  5. extractionAfter a extraction of the aqueous phase with dichlormethane
  6. dry with materialthe combined organic layer was dried over anhydrous sodium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customThe crude product was purified by silica gel chromatography (cyclohexane:ethyl acetate 40:60)

Quellen und Nachweise

ORD-Eintrag
ord-70139663ca2642c695959b34bd86fff4
Quelldatensatz
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08524737B2

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