摘要 |
1-Bromo-4-chlorobutane is prepared by the addition of bromine to a mixture of phosphorus and d -chlorobutanol, the temperature of the mixture being held, during the addition of bromine, to a value close to 0 DEG C. The 1-bromo-4-chlorobutane is preferably separated from the reaction mixture by steam distillation, dried by azeotropic distillation and redistilled in presence of an organic base such as diethanolamine. The d -chlorobutanol is preferably prepared either by the action of gaseous hydrochloric acid on boiling tetrahydrofuran or by heating tetrahydrofuran under reflux with aqueous hydrochloric acid; the raw product from the first method being sufficiently pure to be mixed directly with the phosphorus. Specification 758,895 is referred to. |