1-Propanol → (3,5,6-Trifluoro-2-pyridyl)hydrazine

HRID 1353111Notes

Reaction equation

HRID 1353111 reaction equation
[F:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([F:9])=[C:4](F)[N:3]=1.O.[NH2:12][NH2:13].C(O)CC>ClC>[F:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([F:9])=[C:4]([NH:12][NH2:13])[N:3]=1

Participants

5

Conditions

Temperature
80 °C

Procedure

23.2 g of the compound obtained in Step 1 and 37.3 ml of hydrazine monohydrate were added to 100 ml of n-propanol, and the resulting mixture was heated to 80° C. for 2 hours. The reaction mixture was distilled under a reduced pressure to remove the solvent. The residue thus obtained was dissolved in 100 ml of chloromethane, washed with water, and dried over anhydrous magnesium sulfate. The dried organic layer was concentrated under a reduced pressure to obtain 21.9 g (yield: 83.8%) of the title compound as a light yellow solid.

Workup

  1. distillationThe reaction mixture was distilled under a reduced pressure
  2. customto remove the solvent
  3. customThe residue thus obtained
  4. washwashed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationThe dried organic layer was concentrated under a reduced pressure

Sources & evidence

ORD record
ord-10643c8201fd4ce6a458cad26198adc2
Source dataset
uspto-grants-2007_05
Patent number
US07220863B2

Reaction notes

Loading…