反应详情

To a solution of 5.8 g (0.25 mol) of sodium metal in 175 ml of absolute ethanol is added, dropwise, 24.4 g (0.27 mol) of 2-methyl-2-propanethiol. The stirred solution is heated for 20 minutes, cooled, and treated in a dropwise manner with 44.8 g (0.25 mol) of 1-bromopinacolone, prepared according to the procedure of J. Am. Chem. Soc., 74, 4507 (1952). This reaction mixture is heated at reflux for 20 minutes, cooled, and poured onto 200 g of ice and water. After being saturated with sodium chloride, the mixture is extracted with four portions of ether. The combined ether extracts are dried over anhydrous magnesium sulfate, filtered, and stripped of solvent. Distillation of the residue through a short Vigreaux column gives the desired product. Properties of this, and similar compounds prepared by substantially the same procedure using the appropriate mercaptans and -haloketones, are given in Table 1.

1. temperatureThe stirred solution is heated for 20 minutes
2. temperaturecooled
3. customprepared
4. temperatureThis reaction mixture is heated
5. temperatureat reflux for 20 minutes
6. temperaturecooled
7. extractionthe mixture is extracted with four portions of ether
8. dry with materialThe combined ether extracts are dried over anhydrous magnesium sulfate
9. filtrationfiltered
10. distillationDistillation of the residue through a short Vigreaux column