Sodium Hydroxide → CID 136342890

HRID 1051767

Reaktionsgleichung

Reaktionsgleichung von HRID 1051767
[Cl:1][C:2]1[C:3]2[C:10]([CH:11]=O)=[CH:9][NH:8][C:4]=2[N:5]=[CH:6][N:7]=1.Cl.[NH2:14][OH:15].[OH-].[Na+]>CCO.O>[Cl:1][C:2]1[C:3]2[C:10]([CH:11]=[N:14][OH:15])=[CH:9][NH:8][C:4]=2[N:5]=[CH:6][N:7]=1

Komponenten

6

Edukt 3

HCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 567638284-Chloro-7H-pyrrolo[2,3-d]pyrimidine-5-carbaldehyde

Produkt 1

HCID 136342890CID 136342890

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittel2×HCID 962WaterLösungsmittel

Versuchsvorschrift

To a suspension of 4-chloro-7H-pyrrolo[2,3-d]pyrimidine-5-carbaldehyde (G-2) (1.17 g, 6.47 mmol, 1.0 eq) and hydroxylamine hydrochloride (0.54 g, 7.77 mmol, 1.2 eq) in EtOH (25 mL), aqueous NaOH solution (0.31 g, 7.77 mmol, 1.2 eq) in H2O (4 mL) is added dropwise. The resulting mixture is stirred at RT for 30 min and then is diluted with a sufficient amount of EtOH to allow stirring for additional 30 min. The solid is collected by filtration, rinsed with H2O and dried in vacuo to afford the product, 4-chloro-7H-pyrrolo[2,3-d]pyrimidine-5-carbaldehyde oxime (G-3) as a mixture of isomers.

Aufarbeitung

  1. additionis added dropwise
  2. stirringto allow stirring for additional 30 min
  3. filtrationThe solid is collected by filtration
  4. washrinsed with H2O
  5. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-f69f528acd4e4e69bb15a87ce363325b
Quelldatensatz
uspto-grants-2016_07
Patentnummer
US09388183B2

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