Acetonitrile → HCID 59865001, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 1-[(3-chloropropyl)oxy]-4-iodobenzene (100 g) and acetonitrile (600 ml) is stirred for about 5 min at 25-35° C., then potassium carbonate (93.07 g) followed by 3,3-dimethylpiperidine (49.53 g) are added over about 10 min. Potassium iodide (2.24 g) is added, then the mixture is stirred for about 15 min, before being heated to 78-82° C. for 22-24 h. The reaction mixture is cooled to 25-35° C., and the solid residue is filtered and washed with acetonitrile (200 ml). The filtrate and washings are concentrated under reduced pressure at 50-60° C. to give a thick liquid which is stirred with n-heptane (100 ml) for about 30 min at 25-30° C. The solution is then cooled to −5 to 10° C. and stirred for about 30 min. The solid is filtered, washed with chilled n-heptane (50 ml, 0-5° C.), then dried at 35-40° C. under vacuum for 6-10 h to give the title compound (97 g).

Provenance & Evidence