反应详情

To a solution of 2-methyl-3-nitroisothiourea (15.0 g) in dimethylsulfoxide (100 ml) was gradually added sodium hydride (oil free 2.9 g) at 5° C., while being stirred for one hour. Thereafter, 2-chloro-5-chloromethyl pyridine (18.0 g) was added to the solution at a temperature in the range of from 5° to 10° C., followed by overnight stirring thereof at room temperature. After the dimethylsulfoxide in the solution was distilled off under reduced pressure, the resulting residue was purified on a chromatographic column (the eluent was a mixture of ethanol and chloroform), so as to obtain the desired 1-(2-chloro-5-pyridylmethyl)-2-methyl-3-nitroisothiourea (2.0 g) having a melting point in the range of from 141° to 143° C.

1. customat 5° C.
2. waitfollowed by overnight
3. stirringstirring
4. customat room temperature
5. distillationAfter the dimethylsulfoxide in the solution was distilled off under reduced pressure
6. customthe resulting residue was purified on a chromatographic column (the eluent
7. additiona mixture of ethanol and chloroform), so as