2,4-Difluoroaniline → HCID 23289840, compound

HRID 366397Notes

Reaction equation

HRID 366397 reaction equation
[F:1][C:2]1[CH:8]=[C:7]([F:9])[CH:6]=[CH:5][C:3]=1[NH2:4].O=[C:11]1[CH2:15][CH2:14][CH2:13][CH:12]1[C:16]#[N:17].[Cl-].[Ca+2].[Cl-]>>[F:1][C:2]1[CH:8]=[C:7]([F:9])[CH:6]=[CH:5][C:3]=1[NH:4][C:11]1[CH2:15][CH2:14][CH2:13][C:12]=1[C:16]#[N:17]

Participants

4

Reactant 3

HCID 97092,4-DifluoroanilineHCID 98930Cyclopentanecarbonitrile, 2-oxo-HCID 5284359Calcium Chloride

Product 1

HCID 23289840HCID 23289840, compound

Procedure

2,4-Difluoro-aniline (2.6 g, 20.0 mmol) (Aldrich Chemicals) cyano-ketone (Example 11) (2.2 g, 20.2 mmol), calcium chloride (2.5 g, 22.5 mmol) and T.H.F. (30 ml) were heated under reflux for 19 hours. After cooling, the mixture was filtered and the solvent evaporated. Kugelrohr distillation (125° C., 0.25 mmHg) gave the product as pale yellow crystals.

Workup

  1. temperature(30 ml) were heated
  2. temperatureunder reflux for 19 hours
  3. temperatureAfter cooling
  4. filtrationthe mixture was filtered
  5. customthe solvent evaporated
  6. distillationKugelrohr distillation (125° C., 0.25 mmHg)

Sources & evidence

ORD record
ord-f9b89f23a3994acf846e31d360fb4bd5
Source dataset
uspto-grants-2000_10
Patent number
US06130228

Reaction notes

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