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Methyl 3-cyclohexyl-1H-indole-6-carboxylate → Methyl 2-bromo-3-cyclohexyl-1H-indole-6-carboxylate

HRID 723630
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 723630
[CH3:1][O:2][C:3]([C:5]1[CH:13]=[C:12]2[C:8]([C:9]([CH:14]3[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]3)=[CH:10][NH:11]2)=[CH:7][CH:6]=1)=[O:4].C1C=C[NH+]=CC=1.[Br:26][Br-]Br>C1COCC1.C(Cl)(Cl)Cl>[CH3:1][O:2][C:3]([C:5]1[CH:13]=[C:12]2[C:8]([C:9]([CH:14]3[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]3)=[C:10]([Br:26])[NH:11]2)=[CH:7][CH:6]=1)=[O:4]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 1

HCID 11230631Methyl 3-cyclohexyl-1H-indole-6-carboxylate

Produkt 1

HCID 11175076Methyl 2-bromo-3-cyclohexyl-1H-indole-6-carboxylateAusbeute 85 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6212ChloroformLösungsmittel2×HCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

Adapting the procedure of L. Chu (Tet. Lett. 1997, 38, 3871) methyl,3-cyclohexyl-6-indole carboxylate (4.65 g, 18.07 mmol) was dissolved in a mixture of THF (80 mL) and CHCl3 (80 mL). The solution was cooled in an ice bath and pyridinium bromide perbromide (pyridine tribromide, 7.22 g, 22.6 mmol, 1.25 equivalent) was added. After stirring for 1.5 h at 0° C., the reaction was judged complete by TLC. It was diluted with CHCl3 (200 mL), washed with 1M NaHSO3 (2×50 mL), saturated aqueous NaHCO3 (2×50 mL) and brine (50 mL). After drying over Na2SO4, the solvent was removed under reduced pressure and the residue crystallized from TBME-hexane. The desired 2-bromoindole derivative was collected by filtration, washed with hexane and dried (3.45 g). Evaporation of mother liquors gave a red solid that was purified by flash chromatography using 15% EtOAc in hexane yielding an additional 3.62 g of pure material. Total yield was 5.17 g (85% yield).

Aufarbeitung

  1. temperatureThe solution was cooled in an ice bath
  2. washwashed with 1M NaHSO3 (2×50 mL), saturated aqueous NaHCO3 (2×50 mL) and brine (50 mL)
  3. dry with materialAfter drying over Na2SO4
  4. customthe solvent was removed under reduced pressure
  5. customthe residue crystallized from TBME-hexane
  6. filtrationThe desired 2-bromoindole derivative was collected by filtration
  7. washwashed with hexane
  8. customdried (3.45 g)
  9. customEvaporation of mother liquors
  10. customgave a red solid that
  11. customwas purified by flash chromatography

Quellen und Nachweise

ORD-Eintrag
ord-91d54078658649779b6b2e77ed766046
Quelldatensatz
uspto-grants-2006_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07141574B2

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