3-(Trifluoromethyl)aniline → HCID 53671598, compound

HRID 654409Notes

Reaction equation

HRID 654409 reaction equation
C(=O)([O-])[O-].[K+].[K+].[NH2:7][C:8]1[CH:9]=[C:10]([C:14]([F:17])([F:16])[F:15])[CH:11]=[CH:12][CH:13]=1>CN(C)C=O>[CH2:9]([NH:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([C:14]([F:15])([F:16])[F:17])[CH:9]=1)[CH:8]=[CH:13][CH3:12]

Participants

4

Reactant 2

HCID 73753-(Trifluoromethyl)anilineHCID 11430Potassium Carbonate

Product 1

HCID 53671598HCID 53671598, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

In 30 ml of dimethylformamide, 1.4 g of anhydrous potassium carbonate and 1.0 g of 1-chloro-2l-butene were added to 1.6 g of 3-aminobenzotrifluoride, followed by stirring for 2 hours from 70° C. to 90° C. After potassium carbonate was filtered off, 100 ml of saturated saline were added and the resulting mixture was extracted with benzene. The extract was dried over anhydrous sodium sulfate, concentrated and then subjected to chromatography on a silica gel column (hexane/ethyl acetate: 35/1, v/v), whereby the intended compound was obtained.

Workup

  1. filtrationAfter potassium carbonate was filtered off
  2. addition100 ml of saturated saline were added
  3. extractionthe resulting mixture was extracted with benzene
  4. dry with materialThe extract was dried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. custom35/1, v/v), whereby the intended compound was obtained

Sources & evidence

ORD record
ord-39a494416f9141589ab69d3be6fc6fca
Source dataset
uspto-grants-1992_07
Patent number
US05131947

Reaction notes

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