Water → 5-Chloro-2-[(3-chloropropyl)thio]pyridine

Temperatur

60 °C

5-Chloropyridine-2-thiol (600 mg, 4.12 mmol) synthesized in Example (119a) was dissolved in methanol (15 mL), and 28% sodium methoxide/methanol solution (0.95 mL, 4.94 mmol) and 1-bromo-3-chloropropane (0.61 mL, 6.18 mmol) were added, followed by stirring at 60° C. for 1.5 hours. The reaction solution was cooled to room temperature, water (40 mL) was added, and extraction was carried out twice with ethyl acetate (40 mL). The organic layer was washed with saturated brine, and subsequently dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and vacuum drying was carried out to afford the desired compound (849 mg, yield 92%) as a colorless oil.

1. temperatureThe reaction solution was cooled to room temperature
2. extractionextraction
3. washThe organic layer was washed with saturated brine
4. dry with materialsubsequently dried over anhydrous magnesium sulfate
5. distillationThe solvent was distilled off under reduced pressure, and vacuum
6. customdrying

ORD-Eintrag

ord-27bfc54786ce4677ab8c05b1d11710a6

Quelldatensatz

uspto-grants-2011_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08017610B2