Methanol → Trifop-methyl

HRID 1155790

Reaktionsgleichung

Reaktionsgleichung von HRID 1155790
[F:1][C:2]([F:23])([F:22])[C:3]1[CH:21]=[CH:20][C:6]([O:7][C:8]2[CH:19]=[CH:18][C:11]([O:12][CH:13]([CH3:17])[C:14]([OH:16])=[O:15])=[CH:10][CH:9]=2)=[CH:5][CH:4]=1.[CH3:24]O.B(F)(F)F>O>[F:1][C:2]([F:22])([F:23])[C:3]1[CH:4]=[CH:5][C:6]([O:7][C:8]2[CH:19]=[CH:18][C:11]([O:12][CH:13]([CH3:17])[C:14]([O:16][CH3:24])=[O:15])=[CH:10][CH:9]=2)=[CH:20][CH:21]=1

Komponenten

5

Edukt 3

HCID 887MethanolHCID 6356Boron trifluorideHCID 181206Trifop

Produkt 1

HCID 94586Trifop-methylAusbeute 74 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

10 g of α-[4-(4-trifluoromethylphenoxy)phenoxy]-propionic acid was reacted with 80 g of methanol in the presence of 5 g of boron trifluoride at 55° to 60° C. for 3 hours. The reaction product was poured into water, and extracted with chloroform. The extract was washed with dilute alkali (i.e., 2-3% NaOH aqueous solution) and water, and dried. Then, the chloroform was evaporated off. The residue was distilled at reduced pressure to afford 7.5 g of the final product having a boiling point of 165° to 167° C./3 mmHg. The yield was 74%.

Aufarbeitung

  1. extractionextracted with chloroform
  2. washThe extract was washed with dilute alkali (i.e., 2-3% NaOH aqueous solution) and water
  3. customdried
  4. customThen, the chloroform was evaporated off
  5. distillationThe residue was distilled at reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-d5143ac1ae4c4b8fb448a01b24e6cac4
Quelldatensatz
uspto-grants-1982_06
Patentnummer
US04332961

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