Hydrochloric Acid → HCID 57559703, Verbindung

HRID 1723956Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1723956
C([O:3][C:4]([C:6]1[CH:7]=[N:8][N:9]([C:11]2[CH:16]=[C:15]([C:17](=[O:36])[NH:18][C:19]3[CH:24]=[C:23]([C:25]([CH3:28])([CH3:27])[CH3:26])[CH:22]=[C:21]([NH:29][S:30]([CH3:33])(=[O:32])=[O:31])[C:20]=3[O:34][CH3:35])[CH:14]=[CH:13][C:12]=2[CH3:37])[CH:10]=1)=[O:5])C.[OH-].[Na+].Cl>CO>[C:25]([C:23]1[CH:22]=[C:21]([NH:29][S:30]([CH3:33])(=[O:31])=[O:32])[C:20]([O:34][CH3:35])=[C:19]([NH:18][C:17]([C:15]2[CH:14]=[CH:13][C:12]([CH3:37])=[C:11]([N:9]3[CH:10]=[C:6]([C:4]([OH:5])=[O:3])[CH:7]=[N:8]3)[CH:16]=2)=[O:36])[CH:24]=1)([CH3:28])([CH3:26])[CH3:27]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 11685140HCID 11685140, Verbindung

Produkt 1

HCID 57559703HCID 57559703, VerbindungAusbeute 91,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

1-[5-(5-tert-butyl-3-methanesulfonylamino-2-methoxy-phenylcarbamoyl)-2-methyl-phenyl]-1H-pyrazole-4-carboxylic acid ethyl ester (Example 2) (900 mg) was suspended in MeOH (7 mL). A solution of 10% sodium hydroxide (33 mL) was added and the reaction stirred 2 h. The solution was acidified with concentrated HCl to a pH of 4 resulting in a suspension. The suspension was cooled in an ice bath and the solids collected by vacuum filtration. The solids were washed with water, dried under vacuum over P2O5 at 50° C. to provide 1-[5-(5-tert-butyl-3-methanesulfonylamino-2-methoxy-phenylcarbamoyl)-2-methyl-phenyl]-1H-pyrazole-4-carboxylic acid (782 mg, 91%) as a white solid.

Aufarbeitung

  1. customresulting in a suspension
  2. temperatureThe suspension was cooled in an ice bath
  3. filtrationthe solids collected by vacuum filtration
  4. washThe solids were washed with water
  5. dry with materialdried under vacuum over P2O5 at 50° C.

Quellen und Nachweise

ORD-Eintrag
ord-8064ad693dd0445aa43d35a5a3d0a21f
Quelldatensatz
uspto-grants-2009_02
Patentnummer
US07485657B2

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