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Diisopropylamine → 6-Chloro-3-methyl[1,2]thiazolo[5,4-b]pyridine

HRID 2390941
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2390941
Cl[C:2]([Cl:12])(OC(=O)OC(Cl)(Cl)Cl)Cl.[CH3:13][C:14]1[C:22]2[C:17](=[N:18]C=[CH:20][CH:21]=2)[S:16][N+:15]=1[O-].C(NC(C)C)(C)C>ClCCl>[Cl:12][C:2]1[N:18]=[C:17]2[S:16][N:15]=[C:14]([CH3:13])[C:22]2=[CH:21][CH:20]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 7912DiisopropylamineHCID 94429TriphosgeneHCID 66702670HCID 66702670, Verbindung

Produkt 1

HCID 146892486-Chloro-3-methyl[1,2]thiazolo[5,4-b]pyridineAusbeute 46 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel3×

Versuchsvorschrift

A solution of triphosgene (190 mmol) in dichloromethane (200 mL) was added dropwise over 20 min to a solution of 3-methylisothiazolo [5,4-b]pyridine-N-oxide (47.4 mmol) in dichloromethane (150 mL) at −20° C. A solution of diisopropylamine (190 mmol) in dichloromethane (200 mL) was added dropwise over 1 h. The reaction mixture was allowed to warm to rt and was maintained for 16 h. The reaction mixture was quenched with water (40 mL) of water and the pH was adjusted to 7 by the addition of 10% sodium hydroxide. The organic layer was washed with water (100 mL). The combined aqueous layers were extracted with dichloromethane (10×100 mL) and the combined organic layers were dried (magnesium sulfate) and concentrated. The residue was purified by chromatography (1/80 ethyl acetate/petroleum ether) to provide 6-chloro-3-methylisothiazolo[5,4-b]pyridine in 46% yield as a colorless solid.

Aufarbeitung

  1. temperaturewas maintained for 16 h
  2. customThe reaction mixture was quenched with water (40 mL) of water
  3. additionthe pH was adjusted to 7 by the addition of 10% sodium hydroxide
  4. washThe organic layer was washed with water (100 mL)
  5. extractionThe combined aqueous layers were extracted with dichloromethane (10×100 mL)
  6. dry with materialthe combined organic layers were dried (magnesium sulfate)
  7. concentrationconcentrated
  8. customThe residue was purified by chromatography (1/80 ethyl acetate/petroleum ether)

Quellen und Nachweise

ORD-Eintrag
ord-3b80c47cb6d4424ea23f47823dfe78bc
Quelldatensatz
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08273891B2

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