Sodium Hydroxide → HCID 135741236, Verbindung

HRID 1053820Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1053820
[CH3:1][C:2]([O:5][C:6]([NH:8][C:9]([C:11]1[CH:20]=[CH:19][C:14]([C:15]([O:17]C)=[O:16])=[CH:13][CH:12]=1)=[NH:10])=[O:7])([CH3:4])[CH3:3].[OH-].[Na+]>CO>[CH3:4][C:2]([O:5][C:6]([NH:8][C:9]([C:11]1[CH:12]=[CH:13][C:14]([C:15]([OH:17])=[O:16])=[CH:19][CH:20]=1)=[NH:10])=[O:7])([CH3:1])[CH3:3]

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 135743590methyl 4-(N-(tert-butoxycarbonyl)carbamimidoyl)benzoate

Produkt 1

HCID 135741236HCID 135741236, VerbindungAusbeute 109,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a solution of the compound prepared in Example 17 (0.20 g, 0.72 mmol) in methanol (10 mL) was added 1 M aqueous sodium hydroxide (5 mL). The reaction was stirred at room temperature for 1 h. The mixture was concentrated and the resulting aqueous residue was diluted with ethyl acetate. The aqueous layer was acidified with 1 M hydrochloric acid to pH 4-5 and extracted with ethyl acetate (2×20 mL). The combined organic extracts were dried and concentrated to give the title compound (0.208 g, >99%) as a white solid.

Aufarbeitung

  1. concentrationThe mixture was concentrated
  2. additionthe resulting aqueous residue was diluted with ethyl acetate
  3. extractionextracted with ethyl acetate (2×20 mL)
  4. customThe combined organic extracts were dried
  5. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-fba6974f0f2b422f81bda3cb43b3af30
Quelldatensatz
uspto-grants-2016_07
Patentnummer
US09394250B2

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