Sodium Hydroxide → 3,4,6-Trichloro-2-pyridinecarboxylic acid

HRID 378785Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 378785
[Cl:1][C:2]1[C:3]([C:10]([O:12]C)=[O:11])=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1[Cl:8].[OH-].[Na+]>CO>[Cl:1][C:2]1[C:3]([C:10]([OH:12])=[O:11])=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1[Cl:8]

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 22677534Methyl 3,4,6-trichloropyridine-2-carboxylate

Produkt 1

HCID 134540383,4,6-Trichloro-2-pyridinecarboxylic acidAusbeute 93,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To methyl 3,4,6-Trichloropicolinate (3.57 g, 14.85 mmol) in 20 mL of methanol was added 1N NaOH (14.85 mL, 14.85 mmol). The reaction mixture was stirred at room temperature for 1 hr and then concentrated to dryness in vacuo. 100 mL each of diethyl ether and H2O were added. Aqueous layer was acidified with 1N HCl until pH=2. Methylene chloride was added and the aqueous phase was extracted with additional CH2Cl2 (2×100 mL). The combined extracts were dried (MgSO4) and concentrated to give 3.13 g of a white solid. 1H NMR(CDCl3): δ 7.50 (s, 1H).

Aufarbeitung

  1. concentrationconcentrated to dryness in vacuo
  2. addition100 mL each of diethyl ether and H2O were added
  3. additionMethylene chloride was added
  4. extractionthe aqueous phase was extracted with additional CH2Cl2 (2×100 mL)
  5. dry with materialThe combined extracts were dried (MgSO4)
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-1b38e812deca4b08b94017f78a7e5129
Quelldatensatz
uspto-grants-2001_10
Patentnummer
US06297197B1

Notizen zur Reaktion

Wird geladen…