Potassium Iodide → HCID 15346372, compound

HRID 1585808Notes

Reaction equation

HRID 1585808 reaction equation
[Cl:1][C:2]1[N:3]([C:11]2[CH:16]=[C:15]([OH:17])[C:14]([Cl:18])=[CH:13][C:12]=2[F:19])[N:4]=[C:5]2[C:10]=1[CH2:9][CH2:8][CH2:7][CH2:6]2.C(=O)([O-])[O-].[K+].[K+].[I-].[K+].Br[CH2:29][C:30]#[N:31]>C(C(CC)=O)C>[Cl:1][C:2]1[N:3]([C:11]2[CH:16]=[C:15]([O:17][CH2:29][C:30]#[N:31])[C:14]([Cl:18])=[CH:13][C:12]=2[F:19])[N:4]=[C:5]2[C:10]=1[CH2:9][CH2:8][CH2:7][CH2:6]2

Participants

6

Reactant 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 11534BromoacetonitrileHCID 1850782-Chloro-5-(3-chloro-4,5,6,7-tetrahydroindazol-2-yl)-4-fluorophenol

Product 1

HCID 15346372HCID 15346372, compound

Reagents, catalysts & solvents 1

HCID 7288Ethyl ketoneSolvent3×

Procedure

4.52 g of 3-chloro-2-(4-chloro-2-fluoro-5-hydroxyphenyl)-4,5,6,7-tetrahydroindazole in 10 ml of diethyl ketone were added dropwise at approximately 20° C. to a suspension of 2.07 g of potassium carbonate and 2.49 g of potassium iodide in 150 ml of diethyl ketone. The reaction mixture was subsequently treated with 1.86 g of bromoacetonitrile in 10 ml of diethyl ketone. After the mixture had been refluxed for 10 hours, it was cooled, and the solvent was then removed. The residue was taken up in water, whereupon the solids formed were removed, washed with water and finally dried under reduced pressure at approximately 20° C. Yield: 3.20 g

Workup

  1. temperatureAfter the mixture had been refluxed for 10 hours
  2. temperatureit was cooled
  3. customthe solvent was then removed
  4. customformed
  5. customwere removed
  6. washwashed with water
  7. customfinally dried under reduced pressure at approximately 20° C

Sources & evidence

ORD record
ord-4acb4efebf8c41b49dbb59c2d4183ae8
Source dataset
uspto-grants-1999_08
Patent number
US05939558

Reaction notes

Loading…