Triethylamine → HCID 178505324, compound

Participants

Reaction Steps

447 ml of methanesulphonyl chloride were added portionwise within 20 minutes while cooling with an ice bath to a mixture of 1157 g of trans-N-(7-chloro-quinolin-4-yl)-4-aminocyclohexanol and 868 ml of triethylamine in 6.1 l of dichloromethane. After a clear solution formed transiently the product began to separate. After 2 hours the mixture was filtered and the filtrate was evaporated to dryness. Filter residue and evaporation residue were combined and triturated. in 8 l of water. The mixture was again filtered, washed with a further 8 l of water and thereafter with 4 l of isopropanol and the product obtained was dried at 50° C./12 mbar. Yield: 2028 g (90%) of trans-N-(7-chloro-quinolin-4-yl)-4-methanesulphonyloxy-cyclohexylamine, m.p.: 154-159° C.

Provenance & Evidence