Chlorosulfonyl isocyanate → HCID 19098295, compound

Participants

Reaction Conditions

Reaction Steps

10 g (0.0257 mol) of the compound from Example III are suspended in 100 ml of THF at 0° C., and 2.5 ml (4 g/0.028 mol) of chlorosulphonyl isocyanate are added, with exclusion of moisture. The mixture is allowed to after-react for 15 minutes, while stirring, 120 ml of glacial acetic acid/water (2/1) are added and the temperature is allowed to rise to room temperature. To bring the reaction to completion, the mixture is heated at 100° C. for a further 15 minutes, during which a uniform solution forms. The solution is evaporated to dryness in vacuo, and the residue is extracted by stirring with 50 ml of water for 15 minutes and recrystallised from THF/ethylene chloride.

Provenance & Evidence