Water → HCID 86753304, compound

HRID 355606Notes

Reaction equation

HRID 355606 reaction equation
[F:1][C:2]([F:13])([F:12])[C:3]1[CH:4]=[CH:5][C:6]([N:9]([CH3:11])[NH2:10])=[N:7][CH:8]=1.[CH3:14][CH:15]([CH3:19])[C:16](=O)[CH3:17].C1(C)C=CC(S(O)(=O)=O)=CC=1.O>C1(C)C(C)=CC=CC=1>[F:13][C:2]([F:1])([F:12])[C:3]1[CH:4]=[CH:5][C:6]([N:9]([CH3:11])[N:10]=[C:16]([CH:15]([CH3:19])[CH3:14])[CH3:17])=[N:7][CH:8]=1

Participants

6

Reactant 4

HCID 962WaterHCID 6101p-Toluenesulfonic acidHCID 112513-Methyl-2-butanoneHCID 27777822-(1-Methylhydrazinyl)-5-(trifluoromethyl)pyridine

Product 1

HCID 86753304HCID 86753304, compound

Reagents, catalysts & solvents 1

HCID 7237O-XyleneSolvent

Procedure

A solution of 1-[5-trifluoromethylpyrid-2-yl]-1-methyl hydrazine (5.9 g; 0.031 mol), 3-methyl-2-butanone (5.6 g; 0.065 mol) and p-toluenesulphonic acid (0.1 g) in xylene (30 ml) was heated under reflux, with water removal (azeotrope), for 7 h. The solution was concentrated to yield an oil which was purified by distillation (70° C./72 mbar) to yield 3-methyl-2-butanone 1-[5-trifluoromethylpyrid-2-yl]-1-methyl hydrazone as a yellow oil (5.8 g; 72%). ##STR15##

Workup

  1. concentrationThe solution was concentrated
  2. customto yield an oil which
  3. distillationwas purified by distillation (70° C./72 mbar)

Sources & evidence

ORD record
ord-e68a99cb397e46adadd6a7ae09f6b5e2
Source dataset
uspto-grants-1998_11
Patent number
US05833885

Reaction notes

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