1-Chloro-4-(4-chlorophenyl)-2-butanol synthesis

Yield:59363-13-2 95.51%

Reaction Conditions:

Stage #1: 1-Chloro-4-(chloromethyl)benzenewith iodine;magnesium in tetrahydrofuran;diethyl ether at 35 - 37; for 1 h;
Stage #2: epichlorohydrin in diethyl ether at 37; for 1.5 h;Temperature;Time;

Steps:

1.1

(1)Take 2kg magnesium, 50ml of diethyl ether and a catalytic amount of iodine, at 35 ° C in order to 3ml / s The rate dropped40kg concentration of 0.27g / ml of benzyl chloride chlorine ether solution, after completion of the drop 37° C under 1 hour togive chlorobenzyl chloride Grignard reagent then slowly dropping 20kg concentration 0Epichlorohydrin ether solution .35g /ml, and 1.5 hours after completion of dropping in at 37 ° C to give The reaction solution at 4 ° C, under conditions ofconstant agitation, in the reaction mixture at a rate of 2ml / s of Was added dropwise a 25% concentration of sulfuric acid, tostop the dropwise addition no solid residue constant agitation 10min After standing 10min separate liquids discard theaqueous phase, the organic phase was 0.01MPa,55 ° C conditions Concentrated under ether to no steamed up, distillationcollected 160 ~ 180 ° C / 10mmHg fractions, dry After drying, to obtain the intermediate product 1 detected by HPLC, theyield was 85.1%, which, Target product, 1chloro4(4chlorophenyl)2butanolin an amount of 95.51%

References:

CN105218455,2016,A Location in patent:Paragraph 0054