1-Butanol → Butyl [3-(trifluoromethyl)phenyl]acetate

HRID 2295908

Reaktionsgleichung

Reaktionsgleichung von HRID 2295908
[CH2:1]([OH:5])[CH2:2][CH2:3][CH3:4].[OH-:6].[K+].Cl[C:9](Cl)(Cl)[CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([C:17]([F:20])([F:19])[F:18])[CH:12]=1>O>[F:18][C:17]([F:20])([F:19])[C:13]1[CH:12]=[C:11]([CH2:10][C:9]([O:5][CH2:1][CH2:2][CH2:3][CH3:4])=[O:6])[CH:16]=[CH:15][CH:14]=1

Komponenten

5

Edukt 3

HCID 2631-ButanolHCID 14797Potassium HydroxideHCID 132558021,1,1-Trichloro-2-(3-trifluoromethylphenyl)ethane

Produkt 1

HCID 13255803Butyl [3-(trifluoromethyl)phenyl]acetate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To 200 ml. of butanol was added 40.3 g. of potassium hydroxide containing about 14% of water, and the mixture was stirred at ambient temperature to obtain a gelatinous mixture. To it was added 20 g. of 1,1,1-trichloro-2-(3-trifluoromethylphenyl)ethane, over about 5 minutes. The mixture was then heated to reflux and stirred at that temperature for 5 hours. It was then cooled and worked up as described in Example 1 above. The major product was distilled at 89°-97° under 0.5-0.7 torr to obtain 12.8 g. of the desired product. It was analyzed by vapor phase chromatography, using a 180-cm. column packed with Chrom G silica gel coated with 1.5% of OV-17 and 1.95% of OV-210, and found to be 94.0% pure.

Aufarbeitung

  1. customto obtain a gelatinous mixture
  2. additionTo it was added 20 g
  3. temperatureThe mixture was then heated
  4. temperatureto reflux
  5. temperatureIt was then cooled
  6. distillationThe major product was distilled at 89°-97° under 0.5-0.7 torr
  7. customto obtain 12.8 g

Quellen und Nachweise

ORD-Eintrag
ord-863845700af7490daeec05472740cc03
Quelldatensatz
uspto-grants-1984_01
Patentnummer
US04426536

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