反应详情

A solution of 64.5 g (0.5 mole) of 1,3-dichloro-2-propanol in 200 ml of methylene chloride was treated with 28.5 g (0.5 mole) of methyl isocyanate and a few drops of triethylamine and allowed to stir at ambient temperature overnight. The solution was concentrated and the residue was dissolved in 200 ml of 95% ethanol and treated with a solution of 33.6 g (0.6 mole) of potassium hydroxide in 300 ml of 95% ethanol. The mixture was stirred at ambient temperature for 3.5 hr and then concentrated. The residue was partitioned between 250 ml of benzene and 100 ml of water. The organic layer was washed successively with 50 ml of a 2N hydrochloric acid solution and 100 ml of brine, dried over anhydrous sodium sulfate and concentrated to give 50.5 g of oil as residue. The oil was subjected to vacuum distillation to yield 36.9 g (49%) of clear oil, b.p. 131°-133° C. at 0.3 mm.

1. concentrationThe solution was concentrated
2. dissolutionthe residue was dissolved in 200 ml of 95% ethanol
3. stirringThe mixture was stirred at ambient temperature for 3.5 hr
4. concentrationconcentrated
5. customThe residue was partitioned between 250 ml of benzene and 100 ml of water
6. washThe organic layer was washed successively with 50 ml of a 2N hydrochloric acid solution and 100 ml of brine
7. dry with materialdried over anhydrous sodium sulfate
8. concentrationconcentrated