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2-Dimethylaminopyridine → tert-Butyl 3-bromo-1H-pyrrolo[3,2-c]pyridine-1-carboxylate

HRID 888752
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 888752
[Br:1][C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[N:8][CH:9]=2)[NH:4][CH:3]=1.CN(C1C=CC=CN=1)C.[O:20](C(OC(C)(C)C)=O)[C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=O>C1COCC1>[C:21]([N:4]1[C:5]2[C:10](=[CH:9][N:8]=[CH:7][CH:6]=2)[C:2]([Br:1])=[CH:3]1)([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:20]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 218852-DimethylaminopyridineHCID 90495Di-tert-butyl dicarbonateHCID 156920303-Bromo-5-azaindole2×

Produkt 1

HCID 57415820tert-Butyl 3-bromo-1H-pyrrolo[3,2-c]pyridine-1-carboxylateAusbeute 122,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Referring now to the Scheme 1 as shown in FIG. 1, a solution of 3.5601 g (18.06 mmol) of 3-bromo-5-azaindole (2) and 0.4651 g (3.8 mmol, 21 mol %) of dimethylaminopyridine (DMAP) in 80 mL of THF was placed in a 250 mL three-neck round-bottom flask equipped with a magnetic stirrer, thermocouple, nitrogen bleed, and cooling ice bath. A total of 4.7769 g (21.88 mmol, 1.2 eq.) of BOC2O was added to the flask at 17° C., and the resulting mixture was stirred until starting 3-bromo-5-azaindole disappeared, as monitored by TLC (generally, overnight stirring at room temperature). The resulting yellow solution was concentrated on rotavap, washed with 100 mL of saturated sodium bicarbonate, and extracted with dichloromethane (3×80 mL). The organic phase was dried over Na2SO4 and concentrated on rotavap to afford 6.57 g of orange solid. This crude material was purified on CombiFlash using hexane/ethyl acetate as eluent to give 5.25 g (97% yield) of n-boc-3-bromo-5-azaindole (3) as a white solid.

Aufarbeitung

  1. customequipped with a magnetic stirrer
  2. temperaturecooling ice bath
  3. customovernight
  4. stirringstirring at room temperature)
  5. concentrationThe resulting yellow solution was concentrated on rotavap
  6. washwashed with 100 mL of saturated sodium bicarbonate
  7. extractionextracted with dichloromethane (3×80 mL)
  8. dry with materialThe organic phase was dried over Na2SO4
  9. concentrationconcentrated on rotavap

Quellen und Nachweise

ORD-Eintrag
ord-2c3aad8420804ba3a17f8c09849c50e8
Quelldatensatz
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08252774B2

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