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Hydrazine → 6-fluoro-3-methyl-1H-indazole

HRID 343140
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 343140
[CH3:1][C:2]([C:4]1[CH:9]=[CH:8][C:7]([F:10])=[CH:6][C:5]=1F)=O.[NH2:12][NH2:13]>CCO>[F:10][C:7]1[CH:6]=[C:5]2[C:4]([C:2]([CH3:1])=[N:12][NH:13]2)=[CH:9][CH:8]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 9321HydrazineHCID 677702,4-Difluoroacetophenone

Produkt 1

HCID 1784343226-fluoro-3-methyl-1H-indazoleAusbeute 68,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel2×

Versuchsvorschrift

In a sealed flask were combined 12.99 g (83.2 mmol) 2,4-Difluoroacetophenone, 8.80 g (274 mmol, 3.3 equiv) Hydrazine and 8.7 mL EtOH and heated at 150° C. for 18 h. The resultant solid is dissolved in 150 mL EtOH, precipitated with 500 mL H2O, cooled, filtered, air and pump dried to give 8.56 g (57.0 mmol) 6-Fluoro-3-methyl-1H-indazole which is used without characterization. The material thus obtained is combined with 6.35 g (62.7 mmol, 1.1 equiv) Et3N and 1.39 g (11.4 mmol, 0.2 equiv) DMAP in 110 mL CH3CN cooled to 0° C. 14.93 g (68.4 mmol, 1.2 equiv) (BOC)2O in 80 mL CH3CN is added dropwise with stirring at 0° C. and the resultant reaction mixture stirred 2 h at 0° C. followed by 18 h at ambient temperature. The solvent is removed in vacuo and the crude material partitioned between EtOAc (200 mL) and H2O (100 mL). The pH is adjusted to 2.0 with 1N HCl, the organic phase separated, dried (MgSO4), filtered and concentrated in vacuo to an orange solid which is purified by filtration through a pad of 60 g silica gel eluted with 1.2 L DCM. The filtrate is concentrated in vacuo to give 12.68 g (50.7 mmol) of 6-Fluoro-3-methyl-indazole-1-carboxylic acid tert-butyl ester as a tan crystalline solid: 1H NMR (CDCl3, 300 MHz) δ7.78 (d, 1H, J=9.8), 7.57 (m, 1H), 7.07 (m, 1H), 2.57 (s, 3H), 1.72 (s, 9H); TLC Rf =0.52 (DCM).

Aufarbeitung

  1. customIn a sealed flask were combined
  2. customprecipitated with 500 mL H2O
  3. temperaturecooled
  4. filtrationfiltered
  5. customair and pump dried

Quellen und Nachweise

ORD-Eintrag
ord-9067b273075a45a9943f7d10cd6197c5
Quelldatensatz
uspto-grants-1999_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05859007

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