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Methanol → Methyl 2-chloro-3-fluoropyridine-4-carboxylate

HRID 1180244
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1180244
[Cl:1][C:2]1[C:3]([F:11])=[C:4]([CH:8]=[CH:9][N:10]=1)[C:5]([OH:7])=[O:6].[CH3:12]O>S(Cl)(Cl)=O.ClCCl>[CH3:12][O:6][C:5](=[O:7])[C:4]1[CH:8]=[CH:9][N:10]=[C:2]([Cl:1])[C:3]=1[F:11]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 887MethanolHCID 27828122-Chloro-3-fluoropyridine-4-carboxylic acid

Produkt 1

HCID 24820381Methyl 2-chloro-3-fluoropyridine-4-carboxylateAusbeute 93,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6344DichloromethaneLösungsmittelHCID 24386Thionyl ChlorideLösungsmittel

Versuchsvorschrift

2-Chloro-3-fluoroisonicotinic acid (3.30 g, 18.8 mmol) was suspended in thionyl chloride (40 ml) and heated under reflux for 2.5 h. The solvent was evaporated and the residue dried by means of azeotropic removal of water with toluene (100 ml) to afford a pale yellow oil. The oil was dissolved in dichloromethane (20 ml) and cooled to 0° C. before methanol (2.42 g, 75.3 mmol) was added dropwise to the solution over 15 min. On complete addition the mixture was allowed to warm to ambient temperature and stirred for 18 h. The solvent was evaporated and the mixture partitioned between water (75 ml) and dichloromethane (100 ml). The aqueous phase was extracted further with dichloromethane (100 ml), the organic layers were combined, washed with brine (75 ml), dried over anhydrous sodium sulphate, filtered and evaporated to give 2-chloro-3-fluoroisonicotinic acid methyl ester (3.32 g, 93%) as a pale yellow solid: δH (360 MHz, CDCl3) 3.99 (3H, s), 7.70 (1H, dd, J 5 and 5), 8.31 (1H, d, J 5).

Aufarbeitung

  1. temperatureheated
  2. temperatureunder reflux for 2.5 h
  3. customThe solvent was evaporated
  4. dry with materialthe residue dried by means of azeotropic removal of water with toluene (100 ml)
  5. customto afford a pale yellow oil
  6. additionwas added dropwise to the solution over 15 min
  7. additionOn complete addition the mixture
  8. customThe solvent was evaporated
  9. customthe mixture partitioned between water (75 ml) and dichloromethane (100 ml)
  10. extractionThe aqueous phase was extracted further with dichloromethane (100 ml)
  11. washwashed with brine (75 ml)
  12. dry with materialdried over anhydrous sodium sulphate
  13. filtrationfiltered
  14. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-7ddd90cc31fb48abb7e16c882e98708c
Quelldatensatz
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07279580B2

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