反应详情

A mixture of 129.0 g of di-sec.-butylamine and 129.0 g of chlorobenzene was reacted with phosgene in accordance with Example 1. When the phosgenation was complete, the mixture was heated under reflux for a further hour, the residual phosgene was then removed by blowing out with nitrogen, and, after the solvent had been removed under a moderate vacuum, the main product was collected by distillation. N,N-di-sec.-butylcarbamoyl chloride was obtained in this manner in a yield of 186.0 g and in a purity of 99.8%. The yield of 100% strength carbamoyl chloride was 185.6 g, corresponding to 96.9% of theory. A residue of 2.5 g (corresponding to 1.2% of the theoretical yield) remained in the distillation flask.

1. temperaturethe mixture was heated
2. temperatureunder reflux for a further hour
3. customthe residual phosgene was then removed
4. customafter the solvent had been removed under a moderate vacuum
5. distillationthe main product was collected by distillation