Ethanol → 1-(2-Chloroethyl)amino-1-methylthio-2-nitroethene

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.

1. additionwas then added
2. customAfter they were subjected to reaction at the same temperature for 2 hours
3. customAfter completion of the reaction
4. customthe solvent was removed by distillation under reduced pressure, and 20 ml of ethyl acetate
5. additionwas added to the resulting residue
6. washafter which the resulting mixture was washed with water
7. dry with materialdried over anhydrous magnesium sulfate
8. customthe solvent was removed by distillation under reduced pressure

ORD record

ord-8435f67ed0eb4da7bea22ac412644142

Source dataset

uspto-grants-1987_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04643849