Acetyl chloride → HCID 20538590, compound

HRID 1065781Notes

Reaction equation

HRID 1065781 reaction equation
[Cl:1][C:2]1[C:3]([NH:12][C:13]2[C:18]([N+:19]([O-:21])=[O:20])=[CH:17][C:16]([C:22]([F:25])([F:24])[F:23])=[C:15]([Cl:26])[C:14]=2[N+:27]([O-:29])=[O:28])=[N:4][CH:5]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1.[C:30](Cl)(=[O:32])[CH3:31]>N1C=CC=CC=1>[C:30]([N:12]([C:3]1[C:2]([Cl:1])=[CH:7][C:6]([C:8]([F:9])([F:10])[F:11])=[CH:5][N:4]=1)[C:13]1[C:18]([N+:19]([O-:21])=[O:20])=[CH:17][C:16]([C:22]([F:25])([F:24])[F:23])=[C:15]([Cl:26])[C:14]=1[N+:27]([O-:29])=[O:28])(=[O:32])[CH3:31]

Participants

4

Reactant 2

HCID 6367Acetyl chlorideHCID 91731Fluazinam

Product 1

HCID 20538590HCID 20538590, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent2×

Procedure

In 20 ml. of pyridine, 2.3 g. of N-(3-chloro-5-trifluoromethyl-2-pyridyl)-2,6-dinitro-3-chloro-4-trifluoromethylaniline (obtained in Preparation 4) was dissolved and a solution of 0.34 g. of acetylchloride in 10 ml. of pyridine was added dropwise to react them at 60° to 70° C. for 2 hours. Pyridine was distilled off from the reaction mixture and the product was separated by a silica gel column with an eluent of n-hexane and ethyl acetate (4:1) and the solvent was distilled off to obtain 0.8 g. of the object compound having the melting point of 75° to 77° C.

Workup

  1. customto react them at 60° to 70° C. for 2 hours
  2. distillationPyridine was distilled off from the reaction mixture
  3. customthe product was separated by a silica gel column with an eluent of n-hexane and ethyl acetate (4:1)
  4. distillationthe solvent was distilled off
  5. customto obtain 0.8 g

Sources & evidence

ORD record
ord-d6934c13b50e440e8b14044ef7c4f548
Source dataset
uspto-grants-1982_05
Patent number
US04331670

Reaction notes

Loading…