Hydrochloric Acid → 2-Chloro-3,5-difluoropyridine

HRID 1505063Notes

Reaction equation

HRID 1505063 reaction equation
F[C:2]1[C:7]([F:8])=[CH:6][C:5]([F:9])=[CH:4][N:3]=1.[ClH:10]>O>[Cl:10][C:2]1[C:7]([F:8])=[CH:6][C:5]([F:9])=[CH:4][N:3]=1

Participants

4

Procedure

To a microwave tube is added 2,3,5-trifluoropyridine (2.0 g, 15 mmol), concentrated HCl (12.5 mL, 150 mmol). The mixture is irradiated with microwave for 30 min at 130° C. The reaction mixture is cooled to ambient temperature, diluted with 100 mL of water, extracted with dichloromethane three times. The organic phase is further washed with brine, dried over Na2SO4 and dried to give 2-chloro-3,5-difluoropyridine as a greenish solid. The compound is used without further purification.

Workup

  1. customThe mixture is irradiated with microwave for 30 min at 130° C
  2. extractionextracted with dichloromethane three times
  3. washThe organic phase is further washed with brine
  4. dry with materialdried over Na2SO4
  5. customdried

Sources & evidence

ORD record
ord-0927dd6229484e1d9f6caf8dfe616a71
Source dataset
uspto-grants-2015_12
Patent number
US09216964B2

Reaction notes

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