HRID614014
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
3.9 g of m-chloro-α,α-dimethylbenzyl isocyanate prepared from the corresponding cyanide in the same way as in Synthesis Example 1, was added to a solution of 1.8 g of N-n-butyl-N-methylamine in 20 ml of benzene and the mixture vigorously stirred. After allowing the mixture to stand overnight, the reaction solution was washed with a 2N aqueous hydrochloric acid solution, a 2N aqueous sodium hydroxide solution and water in that order, and the organic layer was dried over sodium sulfate. The layer was concentrated by evaporating off the solvent to obtain crystals, which were recrystallized from n-hexane to obtain 5.0 g of the title compound as crystals.
WORKUP
后处理
- washthe reaction solution was washed with a 2N aqueous hydrochloric acid solution
- dry with materiala 2N aqueous sodium hydroxide solution and water in that order, and the organic layer was dried over sodium sulfate
- concentrationThe layer was concentrated
- customby evaporating off the solvent
- customto obtain crystals, which
- customwere recrystallized from n-hexane