反応 #323438

反応方程式

ethanol

1-methylsulfinyl-1-methylthio-2-nitroethene

2-chloroethylamine hydrochloride

→

1-(2-chloroethyl)amino-1-methylthio-2-nitroethene

収率 57.6%

溶媒

triethylamine

反応条件

後処理

1. 1
   workup.ADDITIONwas then added
2. 2
   その他After they were subjected to reaction at the same temperature for 2 hours
3. 3
   その他After completion of the reaction
4. 4
   その他the solvent was removed by distillation under reduced pressure, and 20 ml of ethyl acetate
5. 5
   workup.ADDITIONwas added to the resulting residue
6. 6
   洗浄after which the resulting mixture was washed with water
7. 7
   乾燥dried over anhydrous magnesium sulfate
8. 8
   その他the solvent was removed by distillation under reduced pressure

実験手順

With 10 ml of ethanol was mixed 1.6 g of 1-methylsulfinyl-1-methylthio-2-nitroethene, and 1.2 g of 2-chloroethylamine hydrochloride was then added thereto, after which 1.0 g of triethylamine was added dropwise at -20° C. in a nitrogen atmosphere. After they were subjected to reaction at the same temperature for 2 hours and then gradually heated to room temperature. After completion of the reaction, the solvent was removed by distillation under reduced pressure, and 20 ml of ethyl acetate was added to the resulting residue, after which the resulting mixture was washed with water and dried over anhydrous magnesium sulfate, and the solvent was removed by distillation under reduced pressure to obtain 1.0 g (yield 54.8%) of 1-(2-chloroethyl)amino-1-methylthio-2-nitroethene having a melting point of 115°-117° C.

出典