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HRID 8481Erstellt: 25. Oktober 2026

Sodium hydride → (3S)-3-Methyl-7,8-difluoro-2,3-dihydro-4H-1,4-benzoxazine

https://huagongshe.com/reaction/8481

Reaktionsgleichung

Beteiligte Stoffe

RolleNameHCIDEinwaage
EduktSodium hydrideHCID 24758—
Edukt(2S)-2-(2,3,4-Trifluoroanilino)propanolHCID 11401466—
LösungsmittelDimethylformamideHCID 6228—
Produkt(3S)-3-Methyl-7,8-difluoro-2,3-dihydro-4H-1,4-benzoxazineHCID 1104142466,5%

Reaktionsbedingungen

Temperatur60 °C

Reaktionsschritte

To DMF (2 ml) was added sodium hydride (39 mg) and the mixture was heated to 60° C. in an oil bath. Next, a solution of the compound (100 mg) obtained in Example 51 in DMF was dropped therein to and the obtained mixture was stirred for 1 hour. After treating in a conventional manner, the mixture was subjected to silica gel column chromatography to give 60 mg (66%) of the title compound. The optical purity determined by HPCL was >94% ee. Various spectral data was identical with those of a specimen synthesized separately.

Herkunft & Nachweise

DOI10.6084/m9.figshare.5104873.v1
PatentnummerUS07087778B2
Quelldatensatzuspto-grants-2006_08
ORD IDord-db2c78a2be8b4889be10b76ac296dc5d
Quellennotizuspto-grants-2006_08