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Benzo(B)Thiophene-2-Boronic Acid → HCID 86710555, Verbindung

HRID 1027162
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1027162
[Cl:1][C:2]1[N:3]=[N:4][C:5](Cl)=[CH:6][CH:7]=1.C([O-])([O-])=O.[Na+].[Na+].[S:15]1[C:19](B(O)O)=[CH:18][C:17]2[CH:23]=[CH:24][CH:25]=[CH:26][C:16]1=2.C(Cl)Cl>COCCOC.O.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[S:15]1[C:19]([C:5]2[N:4]=[N:3][C:2]([Cl:1])=[CH:7][CH:6]=2)=[CH:18][C:17]2[CH:23]=[CH:24][CH:25]=[CH:26][C:16]1=2
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 2359Benzo(B)Thiophene-2-Boronic AcidHCID 6344DichloromethaneHCID 10340Sodium CarbonateHCID 673313,6-Dichloropyridazine

Produkt 1

HCID 86710555HCID 86710555, VerbindungAusbeute 34 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
Katalysator
HCID 962WaterLösungsmittel
HCID 80711,2-DimethoxyethaneLösungsmittel

Reaktionsbedingungen

Temperatur
85 °C

Versuchsvorschrift

To 3,6-dichloropyridazine (4.18 g, 28.1 mmol) and Na2CO3 (8.93 g, 84 mmol) in DME (100 mL) and water (25 mL) was added benzo[b]thiophen-2-ylboronic acid (5 g, 28.1 mmol) and PdCl2(dppf).CH2Cl2 (0.69 g, 0.84 mmol). The reaction was evacuated under vacuum and purged with N2 3×. The reaction was heated at 85° C. for 18 h and cooled to RT. The crude product was filtered through celite and was rinsed with EtOAc followed by CH2Cl2. The crude filtrate was concentrated under vacuum and diluted in CH2Cl2 and water. The organic layer was separated, and the remaining emulsion was acidified with 1 M HCl and extracted with EtOAc. The combined organic layers were washed with water, brine, dried over MgSO4, filtered, and concentrated. The crude product was purified by silica gel chromatography. The product was partially concentrated to provide a precipitate which was filtered to give 3-(benzo[b]thiophen-2-yl)-6-chloropyridazine (2.36 g) as a light yellow solid. The filtrate was recrystallized from CH3CN to give 3-(benzo[b]thiophen-2-yl)-6-chloropyridazine (0.46 g). LCMS Rt=1.57 minutes (condition B); (M+1)=247.1.

Aufarbeitung

  1. customThe reaction was evacuated under vacuum
  2. custompurged with N2 3×
  3. temperaturecooled to RT
  4. filtrationThe crude product was filtered through celite
  5. washwas rinsed with EtOAc
  6. concentrationThe crude filtrate was concentrated under vacuum
  7. additiondiluted in CH2Cl2
  8. customThe organic layer was separated
  9. extractionextracted with EtOAc
  10. washThe combined organic layers were washed with water, brine
  11. dry with materialdried over MgSO4
  12. filtrationfiltered
  13. concentrationconcentrated
  14. customThe crude product was purified by silica gel chromatography
  15. concentrationThe product was partially concentrated
  16. customto provide a precipitate which
  17. filtrationwas filtered

Quellen und Nachweise

ORD-Eintrag
ord-e3bcb258db404b11981b69014f1ff9db
Quelldatensatz
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08729263B2

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