Methyl 3-cyano-2,4,5-trifluoro-benzoate → 195532-64-0

HRID 367014Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 367014
[C:1]([C:3]1[C:4]([F:15])=[C:5]([CH:10]=[C:11]([F:14])[C:12]=1[F:13])[C:6]([O:8]C)=[O:7])#[N:2]>C(O)(=O)C.O.S(=O)(=O)(O)O>[C:1]([C:3]1[C:4]([F:15])=[C:5]([CH:10]=[C:11]([F:14])[C:12]=1[F:13])[C:6]([OH:8])=[O:7])#[N:2]

Komponenten

5

Edukt 1

HCID 18417526Methyl 3-cyano-2,4,5-trifluoro-benzoate

Produkt 1

HCID 18417533195532-64-0Ausbeute 81,3 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 176Acetic AcidLösungsmittelHCID 962WaterLösungsmittelHCID 1118Sulfuric AcidLösungsmittel

Versuchsvorschrift

A solution of 156 g of methyl 3-cyano-2,4,5-trifluoro-benzoate in 960 ml of glacial acetic acid, 140 ml of water and 69 ml of concentrated sulphuric acid is heated to reflux for 8 hours. The acetic acid is then largely removed by distillation in vacuo and the residue is treated with water. The precipitated solid is filtered off with suction, washed with water and dried. 118.6 g of 3-cyano-2,4,5-trifluoro-benzoic acid are obtained as a white solid of melting point 187-190° C.

Aufarbeitung

  1. temperatureto reflux for 8 hours
  2. customThe acetic acid is then largely removed by distillation in vacuo
  3. additionthe residue is treated with water
  4. filtrationThe precipitated solid is filtered off with suction
  5. washwashed with water
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-76c93e836d2145519411fcf0082963d5
Quelldatensatz
uspto-grants-2000_10
Patentnummer
US06133260

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