Water → HCID 10001566, Verbindung

To a solution of 0.125 mL (1.1 mmol) ethyl 2-mercapto-acetate in 2.4 mL dimethylformamide is added 0.68 mL (1.1 mmol) of 1.61 M potassium t-butoxide in tetrahydrofuran. The solution is stirred at room temperature for 30 minutes and then a solution of 0.402 g (0.87 mmol) 5-tosyloxy-8-(3-pyridyl)-1-(2-tetrahydropyranyloxy)-octane in 1 mL dimethylformamide is added. The mixture is stirred at room temperature for 18 hours, poured into water and then extracted with ethyl acetate. The organic phase is washed with water, brine, dried, filtered and evaporated to give an orange oil which is purified by preparative thin layer chromatography using ether, hexane (4:1) as the eluent to give ethyl 8-(2-tetrahydropyranyloxy)-4-[3-(3-pyridyl)propyl]-3-thia-octanoate; IR (CH2Cl2): 1729, 1134 cm-1.

1. stirringThe mixture is stirred at room temperature for 18 hours
2. extractionextracted with ethyl acetate
3. washThe organic phase is washed with water, brine
4. customdried
5. filtrationfiltered
6. customevaporated
7. customto give an orange oil which
8. customis purified by preparative thin layer chromatography

ORD-Eintrag

ord-a50516fadc0a4237802e976bbbdfad83

Quelldatensatz

uspto-grants-1991_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05025025