Methylhydrazine → HCID 86707218, compound

HRID 2408229Notes

Reaction equation

HRID 2408229 reaction equation
[Br:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([C:9](=O)[CH:10]=[CH:11][N:12](C)[CH3:13])=[C:4]([F:16])[CH:3]=1.C[NH:18]N>CO>[Br:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([C:9]2[CH:10]=[CH:11][N:12]([CH3:13])[N:18]=2)=[C:4]([F:16])[CH:3]=1

Participants

4

Reactant 2

HCID 6061MethylhydrazineHCID 86707217HCID 86707217, compound2×

Product 1

HCID 86707218HCID 86707218, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A mixture of 1-(4-bromo-2,6-difluorophenyl)-3-(dimethylamino)-2-propene-1-one (i.e. the product of Step A, 2.39 g, 8.24 mmol) and methylhydrazine (0.42 g, 9.05 mmol) in methanol (50 mL) was stirred at room temperature overnight. The reaction mixture was then concentrated under reduced pressure, and the residue was purified by medium pressure liquid chromatography on silica gel eluted with 0 to 100% ethyl acetate in hexanes to yield the title compound (0.86 g).

Workup

  1. concentrationThe reaction mixture was then concentrated under reduced pressure
  2. customthe residue was purified by medium pressure liquid chromatography on silica gel
  3. washeluted with 0 to 100% ethyl acetate in hexanes

Sources & evidence

ORD record
ord-97edef35f0e34ee9ba9b3fb1f5f44504
Source dataset
uspto-grants-2014_08
Patent number
US08815772B2

Reaction notes

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