Water → HCID 14517625, Verbindung

HRID 2352452Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2352452
[Cl:1][C:2]1[N:3]([C:11]2[C:12]([F:22])=[CH:13][C:14]3[O:19][CH2:18][C:17](=[O:20])[NH:16][C:15]=3[CH:21]=2)[N:4]=[C:5]2[C:10]=1[CH2:9][CH2:8][CH2:7][CH2:6]2.[H-].[Na+].[CH2:25](I)[CH3:26].O>CN(C)C=O>[Cl:1][C:2]1[N:3]([C:11]2[C:12]([F:22])=[CH:13][C:14]3[O:19][CH2:18][C:17](=[O:20])[N:16]([CH2:25][CH3:26])[C:15]=3[CH:21]=2)[N:4]=[C:5]2[C:10]=1[CH2:9][CH2:8][CH2:7][CH2:6]2

Komponenten

6

Edukt 4

HCID 962WaterHCID 6340IodoethaneHCID 24758Sodium hydrideHCID 14517660HCID 14517660, Verbindung

Produkt 1

HCID 14517625HCID 14517625, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a solution of 3-chloro-2-[7-fluoro-2H-1,4-benzoxazin-3(4H)-on-6-yl]-4,5,6,7-tetrahydro-2H-indazole (1.0 g) in N,N-dimethylformamide (10 ml), sodium hydride (0.3 g) and ethyl iodide (0.5 g) were successively added, and the resultant mixture was heated at 50° to 60° C., followed by stirring for 3 hours. The reaction mixture was poured into water, and the precipitated crystals were collected by filtration and purified by silica gel column chromatography using a mixture of ethyl acetate and hexane as an eluent to give Compound No. 1 (0.9 g), m.p., 101.5°-102.5° C.

Aufarbeitung

  1. filtrationthe precipitated crystals were collected by filtration
  2. custompurified by silica gel column chromatography
  3. additiona mixture of ethyl acetate and hexane as an eluent
  4. customto give Compound No
  5. custom101.5°-102.5° C.

Quellen und Nachweise

ORD-Eintrag
ord-6e6097e88df64cb6b2bb551846c0827a
Quelldatensatz
uspto-grants-1989_10
Patentnummer
US04877444

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