Hydrochloric Acid → HCID 765906, Verbindung

HRID 1882946Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1882946
[C:1]([C:5]1[CH:23]=[CH:22][C:8]([C:9]([NH:11][C:12]2[CH:21]=[CH:20][CH:19]=[CH:18][C:13]=2[C:14]([O:16]C)=[O:15])=[O:10])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].C1COCC1.[OH-].[Li+].Cl>CO>[C:1]([C:5]1[CH:23]=[CH:22][C:8]([C:9]([NH:11][C:12]2[CH:21]=[CH:20][CH:19]=[CH:18][C:13]=2[C:14]([OH:16])=[O:15])=[O:10])=[CH:7][CH:6]=1)([CH3:4])([CH3:2])[CH3:3]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 772645HCID 772645, Verbindung

Produkt 1

HCID 765906HCID 765906, VerbindungAusbeute 98 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A stirring solution of methyl 2-(4-tert-butylbenzoyl-amino)benzoate (10.4 g, 33.4 mmol) and THF (200 mL) was treated with 1 M aqueous lithium hydroxide (40 mL) and methanol (80 mL). After stirring over night at room temperature, the mixture was treated with 1 M aqueous HCl (40 mL) and the solvent was removed in vacuo. The residue was partitioned between ethyl acetate (400 mL) and brine (100 mL). The organic phase was separated, then dried with MgSO4, filtered and concentrated in vacuo to give 9.69 g (98%) of a white powder.

Aufarbeitung

  1. customthe solvent was removed in vacuo
  2. customThe residue was partitioned between ethyl acetate (400 mL) and brine (100 mL)
  3. customThe organic phase was separated
  4. dry with materialdried with MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-2602ed5e26304d29a755808754d1353c
Quelldatensatz
uspto-grants-2004_07
Patentnummer
US06759414B2

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