Thioglycerol → 6,7Dihydroxy-3methyl-4-thiaheptanoic acid t-butyl ester

Temperatur

60 °C

To thioglycerol (0.835 ml), t-butyl crotonate (10 ml) and triethylamine (1 ml) were added, followed by stirring at 60° C. for 48 hours. After cooling and addition of water, the reaction mixture was extracted with ethyl acetate. The extract was washed with a 5% aqueous solution of citric acid, a saturated aqueous solution of sodium hydrogen carbonate and saturated saline, and dried over anhydrous sodium sulfate, and the solvent was distilled off, to yield the title compound (1.82 g, yield 73%) as a colorless oily substance.

1. temperatureAfter cooling
2. extractionthe reaction mixture was extracted with ethyl acetate
3. washThe extract was washed with a 5% aqueous solution of citric acid
4. dry with materiala saturated aqueous solution of sodium hydrogen carbonate and saturated saline, and dried over anhydrous sodium sulfate
5. distillationthe solvent was distilled off

ORD-Eintrag

ord-8f641081fb3b4fbf8f3b3c0e8fc51e3e

Quelldatensatz

uspto-grants-1996_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05506267