Water → HCID 21851602, compound

Participants

Reaction Steps

13.6 g of trans-4-(7-chloro-quinolin-4-ylamino)-cyclohexanol (Example 123, step 1) were dissolved in 100 ml of dimethyl sulphoxide and 68 ml of triethylamine and cooled to +10° C. under argon. A solution of 25.5 g of sulphur trioxide-pyridine complex in 100 ml of dimethyl sulphoxide was added dropwise in such a manner that the internal temperature did not exceed +15° C. After stirring for an additional 90 minutes, 800 ml of water were rapidly added dropwise. The emulsion obtained became a filterable suspension after vigourous stirring at +10° C. The filter material was recrystallized from ethanol-ether. Yield: 10.1 g (75%) of beige crystals; dec. 195° C.

Provenance & Evidence