反应详情

To a solution of sodium ethoxide prepared from 7.7 g (0.33 mol) of sodium metal and 200 ml of absolute alcohol was added 19 g (0.4 mol) of methanethiol over 10 min. at ±2° C. To this solution of thiomethoxide was added dropwise, over 25 min., 59 g (0.28 mol) of 1-bromo-3,3-dimethyl-2-butanone prepared according to the procedure of J. Am. Chem. Soc. 74, 4507 (1952). The temperature was maintained at 0°±3° C. during the addition and for a further 30 min. The reaction mixture was filtered and the solvent removed by distillation. Vacuum distillation of the residue gave the desired product as a colorless liquid, b. 73° C./9.3 mm Hg, nD24 1.4650 in 54 percent pure yield.

1. temperatureThe temperature was maintained at 0°±3° C. during the addition and for a further 30 min
2. filtrationThe reaction mixture was filtered
3. customthe solvent removed by distillation
4. distillationVacuum distillation of the residue