Ethyl Acetate → HCID 22912794, compound

HRID 1653948Notes

Reaction equation

HRID 1653948 reaction equation
[Cl:1][C:2]1[C:3]([NH:12][NH2:13])=[N:4][N:5]([CH3:11])[C:6]=1[C:7]([F:10])([F:9])[F:8].C(O[CH:17]=[C:18]([C:21]#[N:22])[C:19]#[N:20])C.C(OCC)(=O)C>C(O)C>[NH2:22][C:21]1[N:12]([C:3]2[C:2]([Cl:1])=[C:6]([C:7]([F:10])([F:8])[F:9])[N:5]([CH3:11])[N:4]=2)[N:13]=[CH:17][C:18]=1[C:19]#[N:20]

Participants

5

Reactant 3

HCID 8857Ethyl AcetateHCID 671522-(Ethoxymethylene)propanedinitrileHCID 22912796HCID 22912796, compound

Product 1

HCID 22912794HCID 22912794, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

1.4 g (6.5 mmole) 4-Chloro-3-hydrazino-1-methyl-5-trifluoromethylpyrazole and 0.81 g (6.5 mmole) ethoxymethylenemalononitrile in 20 ml ethanol were stirred for 10 hours at room temperature and for 2 hours at 50° C. After addition of 100 ml ethyl acetate, the mixture was washed with saturated sodium hydrogen carbonate, dried over sodium sulfate and concentrated. The crude product was purified by silica gel column chromatography (methylene chloride).

Workup

  1. washthe mixture was washed with saturated sodium hydrogen carbonate
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated
  4. customThe crude product was purified by silica gel column chromatography (methylene chloride)

Sources & evidence

ORD record
ord-c386763985954bad83d6d5b296b4c300
Source dataset
uspto-grants-1995_04
Patent number
US05405829

Reaction notes

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