HCID 86746830, compound → HCID 19763431, compound

HRID 248353Notes

Reaction equation

HRID 248353 reaction equation
[Cl:1][C:2]1[CH:3]=[C:4]([NH:22]C(C)=O)[CH:5]=[C:6]([C:18]([F:21])([F:20])[F:19])[C:7]=1[O:8][C:9]([F:17])([F:16])[CH:10]([F:15])[C:11]([F:14])([F:13])[F:12]>Cl.C(O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH:5]=[C:6]([C:18]([F:19])([F:20])[F:21])[C:7]=1[O:8][C:9]([F:16])([F:17])[CH:10]([F:15])[C:11]([F:14])([F:13])[F:12])[NH2:22]

Participants

4

Reactant 1

HCID 86746830HCID 86746830, compound

Product 1

HCID 19763431HCID 19763431, compound

Reagents, catalysts & solvents 2

HCID 313Hydrochloric AcidSolventHCID 702EthanolSolvent

Procedure

42.2 g of 3-chloro-4-(1,1,2,3,3,3-hexafluoropropoxy)-5-(trifluoromethyl)acetaminobenzene are boiled for 16 hours at reflux in a mixture of 200 ml of concentrated hydrochloric acid and 400 ml of ethanol. The bulk of the solvent is then distilled off and the residue is made alkaline and extracted with ether. The ethereal extract is dried over sodium sulfate and the solvent is removed by evaporation in vacuo. Fractional distillation of the residue, affords the title compound as a yellowish oil with a boiling point of 115°-120° C./4·10-2 torr (a compound of formula II).

Workup

  1. distillationThe bulk of the solvent is then distilled off
  2. extractionextracted with ether
  3. extractionThe ethereal extract
  4. dry with materialis dried over sodium sulfate
  5. customthe solvent is removed by evaporation in vacuo
  6. distillationFractional distillation of the residue

Sources & evidence

ORD record
ord-4b64f65ab0af46e1a90587cf490ce2d1
Source dataset
uspto-grants-1993_05
Patent number
US05210100

Reaction notes

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