StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

tert-Butanol → 4-[(6-Chloropyridin-3-yl)methyl]-6-hydroxy-6-hydroxymethyl-5,6,7,7a-tetrahydrofuro[3,2-b]pyridin-2(4H)-one

HRID 552904
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 552904
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][N:9]2CC(=C)C[CH:11]3[O:16][C:17](=[O:19])[CH:18]=[C:10]23)=[CH:4][CH:3]=1.C[N+]1([O-])CC[O:24]CC1.[C:28]([OH:32])([CH3:31])([CH3:30])[CH3:29]>O1CCCC1.[Os](=O)(=O)(=O)=O>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][N:9]2[CH2:30][C:28]([OH:32])([CH2:31][OH:24])[CH2:29][CH:11]3[O:16][C:17](=[O:19])[CH:18]=[C:10]23)=[CH:4][CH:3]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 6386tert-ButanolHCID 82029Methyl morpholine oxideHCID 577798304-[(6-chloropyridin-3-yl)methyl]-6-methylene-5,6,7,7a-tetrahydrofuro[3,2-b]pyridin-2(4H)-one

Produkt 1

HCID 577798284-[(6-Chloropyridin-3-yl)methyl]-6-hydroxy-6-hydroxymethyl-5,6,7,7a-tetrahydrofuro[3,2-b]pyridin-2(4H)-one

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 30318
Osmium Tetroxide
Katalysator
HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

1.86 g (6.72 mmol) of 4-[(6-chloropyridin-3-yl)methyl]-6-methylene-5,6,7,7a-tetrahydrofuro-[3,2-b]pyridin-2(4H)-one (cf. I-5) are dissolved in 20 ml of tetrahydrofuran, and 5.06 ml (0.40 mmol) of a 2.5% strength solution of osmium tetroxide in tert-butanol and 1.28 g (10.08 mmol) of N-methylmorpholine N-oxide are added successively at 0° C. After 3 hours of stirring at room temperature, the mixture is substantially concentrated under reduced pressure, the residue is taken up in water and the mixture is extracted repeatedly with ethyl acetate. Concentration of the organic phase under reduced pressure gives 1.8 g of crude product (mixture of diastereomers). 200 mg of the crude product (taken into account for the determination of the yield) are purified by column chromatography on silica gel (silica gel 60, Merck, particle size: 0.04 to 0.063 mm) using the mobile phase mixture dichloromethane:methanol (95:5 to 90:10). This gives both possible diastereomers of 4-[(6-chloropyridin-3-yl)methyl]-6-hydroxy-6-hydroxymethyl-5,6,7,7a-tetrahydrofuro[3,2-b]pyridin-2(4H)-one: (a) 41 mg (18% of theory) of diastereomer A and (b) 104 mg (47% of theory) of diastereomer B.

Aufarbeitung

  1. concentrationthe mixture is substantially concentrated under reduced pressure
  2. extractionthe mixture is extracted repeatedly with ethyl acetate
  3. customConcentration of the organic phase under reduced pressure gives 1.8 g of crude product (mixture of diastereomers)
  4. customyield)
  5. customare purified by column chromatography on silica gel (silica gel 60, Merck, particle size: 0.04 to 0.063 mm)

Quellen und Nachweise

ORD-Eintrag
ord-f4c5e6a1237c4158b0bb06cd8ab50a40
Quelldatensatz
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07951951B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion