1-Methylthio-1-methylamino-2-nitroethylene → HCID 70002899, compound

HRID 1059457Notes

Reaction equation

HRID 1059457 reaction equation
[NH2:1][CH2:2][C:3]1[CH:4]=[CH:5][C:6]2[S:11][C:10]3[N:12]=[CH:13][CH:14]=[N:15][C:9]=3[NH:8][C:7]=2[CH:16]=1.[CH3:17][NH:18][C:19](SC)=[CH:20][N+:21]([O-:23])=[O:22]>O1CCCC1.O>[N:15]1[C:9]2[NH:8][C:7]3[CH:16]=[C:3]([CH2:2][NH:1][C:19]([NH:18][CH3:17])=[CH:20][N+:21]([O-:23])=[O:22])[CH:4]=[CH:5][C:6]=3[S:11][C:10]=2[N:12]=[CH:13][CH:14]=1

Participants

5

Reactant 2

HCID 1235491-Methylthio-1-methylamino-2-nitroethyleneHCID 18670209HCID 18670209, compound

Product 1

HCID 70002899HCID 70002899, compoundYield 13.9%

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 8028TetrahydrofuranSolvent

Conditions

Temperature
60 °C

Procedure

0.7 g of 8-aminomethyl-10H-pyrazino[2,3-b][1,4]-benzothiazine and 1.35 g of N-methyl-1-methylthio-2-nitro-1-ethenamine were dissolved in a solvent mixture of tetrahydrofuran (50 ml) with water (3 ml) and stirred at 60° C. for 8 hours. After filtering off the insoluble matters, the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluted with methanol/dichloromethane) to thereby give 0.14 g of the title compound as yellow crystals.

Workup

  1. filtrationAfter filtering off the insoluble matters
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe residue was purified by silica gel column chromatography (eluted with methanol/dichloromethane)

Sources & evidence

ORD record
ord-e996ad9deea54390906ad17456b84c6c
Source dataset
uspto-grants-2003_02
Patent number
US06518423B1

Reaction notes

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