Sodium Hydroxide → 2-Ethynyl-5-fluoropyridine

Temperatur

120 °C

820 mg (4.58 mmol) of Dimethylhydroxymethyl-5-fluoro-2-pyridylacetylene and 192 mg (4.81 mmol) of NaOH (KISHIDA CHEMICAL CO., Ltd., 0.7 mm granular, 98%) were placed in a 50 mL two-neck flask equipped with a reflux condenser and the air inside the flask was replaced with Ar. 23 mL of toluene was added thereto and the mixture was refluxed at 120° C. for 0.25 hour. Toluene was added to the reaction mixture and the mixture was washed with a saturated aqueous ammonium chloride solution and dried over magnesium sulfate. The solvent was distilled off under reduced pressure at 90 mmHg/70° C. to give 5-fluoro-2-pyridylethyne as an orange-color liquid (0.35 g, yield: 63%).

1. customequipped with a reflux condenser
2. washthe mixture was washed with a saturated aqueous ammonium chloride solution
3. dry with materialdried over magnesium sulfate
4. distillationThe solvent was distilled off under reduced pressure at 90 mmHg/70° C.

ORD-Eintrag

ord-b616b41a5165482b91a4c56b19786f92

Quelldatensatz

uspto-grants-2012_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08137821B2