Water → HCID 14517625, Verbindung

HRID 1031765Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1031765
[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 an 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. customan purified by silica gel column chromatography
  3. additiona mixture of ethyl acetate and hexane as an eluent
  4. customto give Compound No
  5. customm.p., 101.5 ° -102.5° C.

Quellen und Nachweise

ORD-Eintrag
ord-a58cbfa61b2145498c23f97ef571043a
Quelldatensatz
uspto-grants-1990_09
Patentnummer
US04954626

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