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2,3-Diaminopyridine → Benzyl (2-aminopyridin-3-yl)carbamate

HRID 547382
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 547382
[NH2:1][C:2]1[C:7]([NH2:8])=[CH:6][CH:5]=[CH:4][N:3]=1.[CH2:9]([O:16][C:17](Cl)=[O:18])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>O1CCCC1.N1C=CC=CC=1>[NH2:1][C:2]1[C:7]([NH:8][C:17](=[O:18])[O:16][CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:6][CH:5]=[CH:4][N:3]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 99562,3-DiaminopyridineHCID 10387Benzyl chloroformate

Produkt 1

HCID 13451701Benzyl (2-aminopyridin-3-yl)carbamate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 16069498Pyridine tetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of 2,3-diaminopyridine in tetrahydrofuran/pyridine (10/1) at 0° C. benzylchloroformate was added dropwise. The suspension was stirred at room temperature and after 2 hours partitioned between water and EtOAc. The organic phase was separated and the aqueous phase was extracted with EtOAc. The combined organic phases were dried over sodium sulfate and the filtrate concentrated to dryness under reduced pressure. To the residue was added Et2O-MeOH and the solid was filtered.

Aufarbeitung

  1. custompartitioned between water and EtOAc
  2. customThe organic phase was separated
  3. extractionthe aqueous phase was extracted with EtOAc
  4. dry with materialThe combined organic phases were dried over sodium sulfate
  5. concentrationthe filtrate concentrated to dryness under reduced pressure
  6. additionTo the residue was added Et2O-MeOH
  7. filtrationthe solid was filtered

Quellen und Nachweise

ORD-Eintrag
ord-4b96f569b809458f94b63f6d610ec9c0
Quelldatensatz
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07939537B2

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