Hydrochloric Acid → HCID 178440157, compound

Participants

Reaction Conditions

Reaction Steps

The compound 2 40 g (126 mmol) obtained in the step 1 was suspended in acetonitrile 400 ml, and the suspension was cooled down under nitrogen atmosphere. To the suspension was added dropwise chlorosulfonyl isocyanate 24.3 g (171 mmol) at -20 to -25° C. for 1 hour. To the mixture was added water 400 ml under 10° C. To the mixture was added concentrated hydrochloric acid 40 ml, and the mixture was stirred at 50° C. for 2 hours. The mixture was cooled down to -10° C. and crystallized at the same temperature for 1 hour. The obtained slurry was filtered, washed with cooled acetonitrile, and dried to yield the compound 3 43.2 g. Yield 83%

Provenance & Evidence