Hydrochloric Acid → HCID 66614346, Verbindung
Reaktionsgleichung
[NH2:1][C:2]1[C:7]([C:8]([O:10]CC)=[O:9])=[CH:6][N:5]=[C:4]([C:13]2[C:21]3[C:16](=[N:17][CH:18]=[CH:19][CH:20]=3)[N:15]([CH2:22][C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=3[F:29])[N:14]=2)[N:3]=1.[OH-].[Na+].Cl>O1CCOCC1>[NH2:1][C:2]1[C:7]([C:8]([OH:10])=[O:9])=[CH:6][N:5]=[C:4]([C:13]2[C:21]3[C:16](=[N:17][CH:18]=[CH:19][CH:20]=3)[N:15]([CH2:22][C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=3[F:29])[N:14]=2)[N:3]=1Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 60 °C
Versuchsvorschrift
1000 mg (2.55 mmol) of ethyl 4-amino-2-[1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl]pyrimidine-5-carboxylate (example 101A) were suspended in 80 ml of dioxane and admixed cautiously with 50.1 ml (948 mmol) of aqueous sodium hydroxide solution (50% by weight). The mixture was then stirred at 60° C. for 4 h and then poured onto 200 ml of ice-water. Concentrated hydrochloric acid was used to cautiously adjust the mixture to pH 2, and the precipitate observed was removed by means of filtration. The precipitate was washed with a little water and finally dried under high vacuum. Thus, 993 mg (approx. 105% of theory, the batch probably still contained small amounts of inorganic salts) of the target compound were obtained.
Aufarbeitung
- customthe precipitate observed was removed by means of filtration
- washThe precipitate was washed with a little water
- customfinally dried under high vacuum
- customThus, 993 mg (approx. 105% of theory, the batch probably still contained small amounts of inorganic salts) of the target compound were obtained
Quellen und Nachweise
- ORD-Eintrag
- ord-1a27d821a8314bc4a846a433d9d38ef1
- Quelldatensatz
- uspto-grants-2015_08
- Patentnummer
- US09096592B2
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