1-Methylthio-1-methylamino-2-nitroethylene → HCID 70018281, compound
Reaction equation
[CH3:1][NH:2][C:3](SC)=[CH:4][N+:5]([O-:7])=[O:6].[F:10][C:11]([F:23])([F:22])[C:12]1[CH:17]=[C:16]([O:18][CH3:19])[N:15]=[C:14]([NH:20][NH2:21])[CH:13]=1>C(O)C>[CH3:1][NH:2][C:3]([NH:21][NH:20][C:14]1[CH:13]=[C:12]([C:11]([F:23])([F:22])[F:10])[CH:17]=[C:16]([O:18][CH3:19])[N:15]=1)=[CH:4][N+:5]([O-:7])=[O:6]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
4.7 g of N-methyl-1-methylthio-2-nitroetheneamine, 6.6 g of crude 4-trifluoromethyl-6-methoxy-2-pyridylhydrazine (Intermediate No. 71) and 35 ml of ethanol were stirred for about 5.5 hours under heating and refluxing and then cooled to room temperature, whereupon precipitated crystals were collected by filtration. The crystals obtained by filtration were washed with a small amount of methanol and then dried to obtain 2.7 g of N-methyl-1-(2-(4-trifluoromethyl-6-methoxy-2-pyridyl)hydrazino)-2-nitroetheneamine (Compound No. 98) having a melting point of 193° C. (decomposed).
Workup
- temperatureunder heating
- temperaturerefluxing
- customwhereupon precipitated crystals
- filtrationwere collected by filtration
- customThe crystals obtained by filtration
- washwere washed with a small amount of methanol
- customdried
Sources & evidence
- ORD record
- ord-b0a750ac47984cefab692fbd80b34fde
- Source dataset
- uspto-grants-2003_07
- Patent number
- US06596863B2
Reaction notes
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