Potassium Iodide → HCID 15124793, compound

Participants

Reaction Steps

A mixture of 93 parts of N-(2-chloroethyl)-N-(3-chloropropyl)-4-methylbenzenesulfonamide, 30.3 parts of 2,3-dimethylbenzenamine, 63.6 parts of sodium carbonate, 1 part of potassium iodide and 240 parts of cyclohexanol was stirred and refluxed over weekend using a water separator. After cooling, the reaction mixture was poured into water. The product was extracted with methylbenzene. The extract was washed twice with water, dried, filtered and evaporated. The residue was crystallized from 2-propanol and a small amount of tetrahydrofuran. The product was filtered off and dried, yielding 47.8 parts (53.3%) of 1-(2.3-dimethylphenyl)hexahydro-4-[(4-methylphenyl)sulfonyl]-1H-1.4-diazepine; mp. 86.2° C. (intermediate 7).

Provenance & Evidence