bromine; triphenylphosphine; n-methylacetamide;
reactants are commercially availlable.
bayer aktiengesellschaft, us6008420, a1, (1999) example 1 (for comparison) 1250 ml of dimethylformamide were placed into the reaction vessel, and then 280.8 g of triphenylphosphine and then 70 g of hydroxymethylcyclopropane were added, the mixture was stirred for 30 minutes at room temperature under a nitrogen atmosphere, and the solution was sub sequently cooled to -10°c. then, 158.3 g of bromine (that is to say 2 mol percent more than theoret ically required) were metered in in the course of 4 hours. the reaction mixture was worked up by distillation. bromomethylcyclopropane was obtained in a yield of 77.5percent of theory. the purity of the product was over 97percent, the open-chain halogenoalkanes amounted to 0.6percent.
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