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Tetrahydrofuran → 6-(DifluoroMethyl)-2-pyridinecarboxylic Acid

HRID 1426288
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1426288
[F:1][CH:2]([F:13])[C:3]1[N:8]=[C:7]([C:9]([O:11]C)=[O:10])[CH:6]=[CH:5][CH:4]=1.O1CCCC1.O.[OH-].[Li+]>O>[F:13][CH:2]([F:1])[C:3]1[N:8]=[C:7]([C:9]([OH:11])=[O:10])[CH:6]=[CH:5][CH:4]=1
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Komponenten

5

Edukt 3

HCID 8028TetrahydrofuranHCID 168937Lithium hydroxide, monohydrateHCID 69673506methyl 6-(difluoromethyl)picolinate

Produkt 1

HCID 696735676-(DifluoroMethyl)-2-pyridinecarboxylic AcidAusbeute 65,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To a solution of methyl 6-(difluoromethyl)pyridine-2-carboxylate (0.58 g, 3.1 mmol, from Step 1) in Water (22 mL) and Tetrahydrofuran (20 mL, 250 mmol) was added Lithium hydroxide, monohydrate (0.65 g, 15 mmol). The reaction was stirred for 2 hours. The basic mixture was extracted with ether, which was discarded. The mixture was then acidified by the addition of 1N HCl and the volume of solvent reduced in vacuo. The product was purified via preparative HPLC-MS (C18, eluting with a gradient of H2O/MeCN containing 0.1% TFA). The eluent containing the desired mass was evaporated by rotary evaporation to afford a solid product (0.35 g, 65%). 1H NMR (400 MHz, CD3OD): δ 8.27 (ddd, 1H), 8.17 (dd, 1H), 7.92 (dd, 1H), 6.78 (t, 1H); 1H NMR (400 MHz, CD3OD): δ−117.52 (d, 2F); LCMS (M+H)+: 173.9.

Aufarbeitung

  1. extractionThe basic mixture was extracted with ether, which
  2. additionThe mixture was then acidified by the addition of 1N HCl
  3. customThe product was purified via preparative HPLC-MS (C18
  4. washeluting with a gradient of H2O/MeCN containing 0.1% TFA)
  5. additionThe eluent containing the desired mass
  6. customwas evaporated by rotary evaporation

Quellen und Nachweise

ORD-Eintrag
ord-b078d962073f43c88ed609df7611a296
Quelldatensatz
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08933085B2

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