Methylhydrazine → 1-Methyl-2-(1-methylsulfonyl-2-propylidene)hydrazine

To a 100 ml volume four-necked flask, 1-methylsulfonyl-2-propanone (7-2-1) (4.99 g) and toluene (36.0 g) were added under a nitrogen atmosphere, and added dropwise 40 wt % of aqueous monomethylhydrazine solution (14-a) (3.96 g) at room temperature. The resulting mixture was stirred at room temperature for 16 hours, and then added additional 40 wt % of aqueous monomethylhydrazine solution (0.35 g). The resulting mixture was stirred for 24 hours, and refluxed with Dean-Stark apparatus under reduced pressure at the internal temperature of 50° C. After refluxing, the resulting mixture was cooled to 0° C., and filtered to give 3.56 g of 1-methyl-2-(1-methylsulfonyl-2-propylidene)hydrazine (5-2-1).

1. stirringThe resulting mixture was stirred for 24 hours
2. temperaturerefluxed with Dean-Stark apparatus under reduced pressure at the internal temperature of 50° C
3. temperatureAfter refluxing
4. temperaturethe resulting mixture was cooled to 0° C.
5. filtrationfiltered

ORD record

ord-d2a0bd8bd54f4a5f9c7adffbbd7849d0

Source dataset

uspto-grants-2015_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09040709B2