Hydrochloric Acid → HCID 7174615, Verbindung

HRID 1054318Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1054318
[CH3:1][C:2]1[C:10]2[C:9]([C:11]([O:13]C)=[O:12])=[CH:8][C:7]([CH3:15])=[N:6][C:5]=2[N:4]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[N:3]=1.Cl>>[CH3:1][C:2]1[C:10]2[C:9]([C:11]([OH:13])=[O:12])=[CH:8][C:7]([CH3:15])=[N:6][C:5]=2[N:4]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[N:3]=1

Komponenten

3

Edukt 2

HCID 313Hydrochloric AcidHCID 17025734methyl 3,6-dimethyl-1-phenylpyrazolo[3,4-b]pyridine-4-carboxylate

Produkt 1

HCID 7174615HCID 7174615, VerbindungAusbeute 81 %

Versuchsvorschrift

Synthesized using the procedure for 1 except ester 46 was used as the starting material. After the work up and acidifying the aqueous layer with 1N HCl, solid precipitated which was filtered off and dried on high vacuum to provide the title compound (165 mg, 81%) as a light yellow solid. 100% pure by HPLC. 1H NMR (400 MHz, DMSO-d6) δ 13.90 (s, 1H), 8.19 (d, J=7.7 Hz, 2H), 7.56-7.48 (m, 3H), 7.29 (t, J=7.3 Hz, 1H), 2.65 (s, 3H), 2.63 (s, 3H). 13C NMR (100 MHz, DMSO-d6) δ 167.04, 159.52, 151.67, 142.43, 139.35, 135.32, 129.49, 126.12, 121.13, 118.29, 111.04, 24.92, 16.12. ESI MS: m/z 268.1 (M+H)+.

Aufarbeitung

  1. customSynthesized
  2. customprecipitated which
  3. filtrationwas filtered off
  4. customdried on high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-fbaebd89cebc4935a66b8e06944e2e76
Quelldatensatz
uspto-grants-2016_07
Patentnummer
US09394303B2

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