反应详情

To a solution of 1-(2-chloro-5-thiazolylmethyl)-3,3- dimethyl-2-nitroguanidine (0.300 g) in an aqueous NaOH solution (NaOH (0.319 g) and water (10 ml)) were added CH2Cl2 (10 ml) and 4-dimethylaminopyridine (0.013 g). To the mixture was added methanesulphonyl chloride (0.391 g) dropwise at room temperature under stirring. After stirring for 30 minutes, the mixture was partitioned. The organic layer was dried over MgSO, and concentrated in vacuo. The resulting residue was applied to column chromatography on silica gel. The column was eluted with hexane-AcOEt (1:1) to afford 0.160 g of 1-(2-chloro-5-thiazolylmethyl)-3,3-dimethyl-l-methanesulphonyl-2-nitroguanidine (Compound No. 28) as a pale yellow crystal, m.p. 82°-86° C.

1. stirringAfter stirring for 30 minutes
2. customthe mixture was partitioned
3. dry with materialThe organic layer was dried over MgSO
4. concentrationconcentrated in vacuo
5. washThe column was eluted with hexane-AcOEt (1:1)