Lithium hydroxide, monohydrate → 3-Iodo-5-(5-methyl-pyridin-2-yl)-benzoic acid

HRID 506636Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 506636
O[Li].O.C[O:5][C:6](=[O:21])[C:7]1[CH:12]=[C:11]([C:13]2[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][N:14]=2)[CH:10]=[C:9]([I:20])[CH:8]=1>O.C1COCC1>[I:20][C:9]1[CH:8]=[C:7]([CH:12]=[C:11]([C:13]2[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][N:14]=2)[CH:10]=1)[C:6]([OH:21])=[O:5]

Komponenten

5

Edukt 2

HCID 168937Lithium hydroxide, monohydrateHCID 594325793-Iodo-5-(5-methyl-pyridin-2-yl)-benzoic acid methyl ester

Produkt 1

HCID 595997013-Iodo-5-(5-methyl-pyridin-2-yl)-benzoic acidAusbeute 100,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A solution of LiOH hydrate (20 mg) in H2O (5 mL) was added dropwise to a suspension of 3-iodo-5-(5-methyl-pyridin-2-yl)-benzoic acid methyl ester (85 mg, 0.2 mmol) in THF (1 mL) at 0° C. The reaction mixture was allowed to warm to room temperature and was stirred until the reaction solution turned clear. Solvent was removed under vacuum and the resulting aqueous solution was acidified by 10% HCl to pH=6-7. The resulting precipitate was collected and dried to afford 3-iodo-5-(5-methyl-pyridin-2-yl)-benzoic acid (68 mg, 95%), MS (M+H)=339.

Aufarbeitung

  1. customSolvent was removed under vacuum
  2. customThe resulting precipitate was collected
  3. customdried

Quellen und Nachweise

ORD-Eintrag
ord-c2ddbbe7ed0c4baeb65cd0ae64fa6805
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07786110B2

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