Iodine → HCID 178474493, Verbindung

HRID 588584Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 588584
[F:1][C:2]([F:13])([F:12])[C:3]1[CH:7]=[C:6]([NH:8][C:9](=[O:11])[CH3:10])[NH:5][N:4]=1.[I:14](O)(=O)=O.II>C(O)C>[I:14][C:7]1[C:3]([C:2]([F:1])([F:12])[F:13])=[N:4][NH:5][C:6]=1[NH:8][C:9](=[O:11])[CH3:10]

Komponenten

5

Edukt 3

HCID 807IodineHCID 24345Iodic acidHCID 178474234HCID 178474234, Verbindung

Produkt 1

HCID 178474493HCID 178474493, VerbindungAusbeute 296,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
65 °C

Versuchsvorschrift

To a solution of N-[3-(trifluoromethyl)-1H-pyrazol-5-yl]acetamide (7.3 g, 38 mmol) in ethanol (120 mL) were added iodic acid (1.65 g, 9.4 mmol) and iodine (4.8 g, 18.9 mmol). The reaction was stirred for 3.25 h at 65° C. The reaction mixture was concentrated in vacuo and the residue was suspended in hot CH2Cl2 (150 ml) with stirring, the solid was filtered and resuspended in hot CH2Cl2 (100 ml) filtered and dried in vacuo to provide the title compound as a white solid (8.9 g) which was used in the subsequent step.

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. stirringwith stirring
  3. filtrationthe solid was filtered
  4. filtrationfiltered
  5. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-383135e79a1244a8aff3053bb178f680
Quelldatensatz
uspto-grants-2016_01
Patentnummer
US09227976B2

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