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Tetrahydrofuran → 4-Benzyloxy-2-((S)-2-hydroxy-propylamino)-benzaldehyde

HRID 1815949
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1815949
[CH2:1]([O:8][C:9]1[CH:16]=[CH:15][C:12]([C:13]#N)=[C:11]([NH:17][CH2:18][C@@H:19]([OH:21])[CH3:20])[CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C1CCCCC1.[H-].C([NH2+]CC(C)C)C(C)C.C1C[O:41]CC1>>[CH2:1]([O:8][C:9]1[CH:16]=[CH:15][C:12]([CH:13]=[O:41])=[C:11]([NH:17][CH2:18][C@@H:19]([OH:21])[CH3:20])[CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 4

HCID 8028TetrahydrofuranHCID 8078CyclohexaneHCID 21898182Diisobutylammonium hydride2×HCID 69564440HCID 69564440, Verbindung

Produkt 1

HCID 867596484-Benzyloxy-2-((S)-2-hydroxy-propylamino)-benzaldehyde

Versuchsvorschrift

To a solution of the product of Step B (19.3 g, 68.3 mmol) in a mixture of anhydrous cyclohexane and THF (200 mL, 40 mL) at 0° C. under nitrogen was added diisobutylammonium hydride (1 M solution in hexane, 239 mL, 239 mmol) over 30 min. This mixture was stirred 18 h at ambient temperature, additional diisobutylammonium hydride (40 mL, 40 mmol) was added, and the mixture was stirred an additional 24 h. The reaction mixture was cooled on an ice bath and the reaction was quenched by the addition of MeOH (exothermic) and 2 N HCl to maintain a pH of 1. The mixture was extracted with EtOAc (3×300 mL) and the extracts were dried and concentrated to a brown oil (18.5 g). The crude oil was triturated with EtOAc/hexane, and filtered to give an oil (16.1 g, 83% crude yield). A small portion of this material was purified by chromatography (silica, 20% to 50% EtOAc/hexane) to afford a solid; mp 68-69° C.

Aufarbeitung

  1. stirringthe mixture was stirred an additional 24 h
  2. temperatureThe reaction mixture was cooled on an ice bath
  3. customthe reaction was quenched by the addition of MeOH (exothermic) and 2 N HCl
  4. temperatureto maintain a pH of 1
  5. extractionThe mixture was extracted with EtOAc (3×300 mL)
  6. customthe extracts were dried
  7. concentrationconcentrated to a brown oil (18.5 g)
  8. customThe crude oil was triturated with EtOAc/hexane
  9. filtrationfiltered
  10. customto give an oil (16.1 g, 83% crude yield)
  11. customA small portion of this material was purified by chromatography (silica, 20% to 50% EtOAc/hexane)
  12. customto afford a solid

Quellen und Nachweise

ORD-Eintrag
ord-b7b8d69bb593466bbc5772fb4fb82242
Quelldatensatz
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06881749B2

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