Potassium Hydroxide → HCID 178506226, Verbindung

2-chloro-5-trifluoromethylpyridine (13.7 g) was dissolved in ethanol (96 ml), thiourea (5.7 g) was added to the mixture, and the mixture was heated to reflux for 3 hours. After allowing the mixture to be cooled to room temperature, an aqueous solution (19.2 ml) of potassium hydroxide (6.4 g) was added to the mixture, and the mixture was heated to reflux for 1 hour. After allowing the mixture to be cooled to room temperature, diluted aqueous solution of potassium hydroxide (20 ml) was added to the mixture, and the mixture was washed with methylene chloride. With acetic acid, pH of the mixture was adjusted to about 6, and the mixture was extracted with methylene chloride. The mixture was washed with water, and dried over magnesium sulfate. The solvent was removed under reduced pressure and the obtained residue was washed with hexane/ethyl acetate, to give 2-mercapto-5-trifluoromethylpyridine (5.1 g).

1. temperaturethe mixture was heated
2. temperatureto reflux for 3 hours
3. temperaturethe mixture was heated
4. temperatureto reflux for 1 hour
5. temperatureto be cooled to room temperature
6. washthe mixture was washed with methylene chloride
7. extractionthe mixture was extracted with methylene chloride
8. washThe mixture was washed with water
9. dry with materialdried over magnesium sulfate
10. customThe solvent was removed under reduced pressure
11. washthe obtained residue was washed with hexane/ethyl acetate

ORD-Eintrag

ord-f88f3e55b9114a3990cea8a2d71ac5b7

Quelldatensatz

uspto-grants-2007_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07262185B2