Formic Acid → HCID 178432647, Verbindung

HRID 2200323Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2200323
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:9](=[NH:12])[NH:10][NH2:11])=[N:6][C:7]=1[CH3:8].[CH:13](O)=O>CO>[Br:1][C:2]1[C:7]([CH3:8])=[N:6][C:5]([C:9]2[NH:12][CH:13]=[N:11][N:10]=2)=[CH:4][CH:3]=1

Komponenten

4

Edukt 2

HCID 284Formic AcidHCID 178432964HCID 178432964, Verbindung

Produkt 1

HCID 178432647HCID 178432647, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

5-Bromo-6-methylpicolin-imido-hydrazide (1 equiv) and formic acid (15 equiv) were combined and heated to 100° C. for 6 h. The reaction was cooled to room temperature and diluted with methanol. The resulting slurry was partially concentrated under reduced pressure and the resulting mixture was diluted with methanol and partially concentrated under reduced pressure. The resulting solids were collected by filtration, washed with water and dried to provide the desired product, as a solid. MS (ESI) m/z 238.9 [M]+, 240.9 [M+2]+.

Aufarbeitung

  1. temperatureThe reaction was cooled to room temperature
  2. concentrationThe resulting slurry was partially concentrated under reduced pressure
  3. additionthe resulting mixture was diluted with methanol
  4. concentrationpartially concentrated under reduced pressure
  5. filtrationThe resulting solids were collected by filtration
  6. washwashed with water
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-91ba00941eff47dd9f320718d2efa8dd
Quelldatensatz
uspto-grants-2016_06
Patentnummer
US09359364B2

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