Sodium Hydroxide → HCID 66621889, Verbindung

HRID 416239

Reaktionsgleichung

Reaktionsgleichung von HRID 416239
[OH-].[Na+].C[O:4][C:5](=[O:21])[C:6]1[CH:11]=[CH:10][C:9]([CH2:12][N:13]2[CH:17]=[C:16]([C:18]#[N:19])[C:15]([NH2:20])=[N:14]2)=[CH:8][CH:7]=1>O.CO>[NH2:20][C:15]1[C:16]([C:18]#[N:19])=[CH:17][N:13]([CH2:12][C:9]2[CH:10]=[CH:11][C:6]([C:5]([OH:21])=[O:4])=[CH:7][CH:8]=2)[N:14]=1

Komponenten

5

Edukt 2

HCID 14798Sodium HydroxideHCID 666222814-(3-Amino-4-cyano-pyrazol-1-ylmethyl)-benzoic acid methyl ester

Produkt 1

HCID 66621889HCID 66621889, VerbindungAusbeute 92,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

To a solution of NaOH (343 mg, 8.58 mmol) in a mixture of water (10 ml) and MeOH (20 ml) the ester 95 (732 mg, 2.86 mmol) was added. The reaction mixture was refluxed 2 min and stirred for additional 2 hrs at ambient temperature. MeOH was removed under reduced pressure and remaining aqueous solution was acidified with conc. HCl (pH 3-4) to form a precipitate which was collected by filtration to afford the title compound (96) (640 mg, 92% yield). LRMS: 242.2 (calc.), 241.1 (found).

Aufarbeitung

  1. additionwas added
  2. temperatureThe reaction mixture was refluxed 2 min
  3. customMeOH was removed under reduced pressure
  4. customto form a precipitate which
  5. filtrationwas collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-d817d97b262047d2a4e275c19967742a
Quelldatensatz
uspto-grants-2012_01
Patentnummer
US08088805B2

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