1-Dodecanethiol → HCID 178442864, compound

Participants

Reaction Steps

In a 1000 ml flask equipped with a stirrer, a condenser and a calcium chloride dryer tube were charged 26.6 g of 11-bromoundecanoic acid, 21.2 g of 1-dodecanthiol, 42.4 ml of sodium methoxide (28% methanol solution) and 300 ml of methanol, and the mixture was refluxed for 6 hours on an oil bath. After cooling the reaction mixture to room temperature, the precipitated crystals were collected by filtration under reduced pressure and washed with methanol. The resulting crystals were suspended in 1000 ml of distilled water, and the suspension was made pH 2 by adding a conc. hydrochloric acid, and suspension was stirred on an oil bath at 60° C. for 30 minutes to carry out neutraliza tion. Crystals after neutralization were collected by filtration under reduced pressure and washed with distilled water. The residue was recrystallized from ethanol to obtain 35.2 g of the title compound.

Provenance & Evidence