Lithium → 7,8-Difluoro-3,4-dihydro-2H-1,4-benzothiazine

HRID 2416850Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2416850
[F:1][C:2]1[CH:12]=[CH:11][C:5]2[NH:6][C:7](=O)[CH2:8][S:9][C:4]=2[C:3]=1[F:13].[Li]>C1COCC1>[F:1][C:2]1[CH:12]=[CH:11][C:5]2[NH:6][CH2:7][CH2:8][S:9][C:4]=2[C:3]=1[F:13]

Komponenten

4

Edukt 2

HCID 3028194LithiumHCID 22632969HCID 22632969, Verbindung

Produkt 1

HCID 226329587,8-Difluoro-3,4-dihydro-2H-1,4-benzothiazineAusbeute 104 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A solution of 7,8-difluoro-4H-benzo[1,4]thiazin-3-one (Example L-3, 2.27 g, 11.3 mmol) in THF (100 mL) was reacted with lithium aluminumhydride (1.07 g, 28.2 mmol) under an N2 atmosphere and heated to reflux overnight. The mixture was cooled and quenched with 1.0N HCl and extracted with ethyl acetate. The organic layers were combined, dried with sodium sulfate, and concentrated to provide 2.2 g of the title compound as an oil.

Aufarbeitung

  1. temperatureheated
  2. temperatureto reflux overnight
  3. temperatureThe mixture was cooled
  4. customquenched with 1.0N HCl
  5. extractionextracted with ethyl acetate
  6. dry with materialdried with sodium sulfate
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-6f517e4540994d20b33bf66295527942
Quelldatensatz
uspto-grants-2004_11
Patentnummer
US06825199B2

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