Hydrochloric Acid → HCID 10568313, Verbindung

HRID 862075Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 862075
[Br:1][C:2]1[C:3]([Cl:24])=[CH:4][C:5]([O:20]COC)=[C:6]([CH:19]=1)[C:7]([C:9]1[C:14]([O:15]COC)=[CH:13][CH:12]=[CH:11][N:10]=1)=[O:8].Cl>CO>[Br:1][C:2]1[C:3]([Cl:24])=[CH:4][C:5]([OH:20])=[C:6]([CH:19]=1)[C:7]([C:9]1[C:14]([OH:15])=[CH:13][CH:12]=[CH:11][N:10]=1)=[O:8]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 108357432-(5-Bromo-4-chloro-2-methoxymethoxybenzoyl)-3-methoxymethoxypyridine

Produkt 1

HCID 10568313HCID 10568313, VerbindungAusbeute 97,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

To a solution of 2-(5-bromo-4-chloro-2-methoxymethoxybenzoyl)-3-methoxymethoxypyridine (7.73 g) in methanol (250 ml) was added hydrochloric acid (12.5 ml), which was stirred for 5 hours at 50° C. Methanol was distilled off under reduced pressure. To the residue was added ethyl acetate (5 ml), which was poured into water. Crystalline precipitate then formed was collected by filtration, washed with ethyl acetate 10 and dried to give 2-(5-bromo-4-chloro-2-hydroxybenzoyl)-3-hydroxypyridine (5.95 g) (Compound A-8).

Aufarbeitung

  1. distillationMethanol was distilled off under reduced pressure
  2. additionTo the residue was added ethyl acetate (5 ml), which
  3. additionwas poured into water
  4. customCrystalline precipitate then formed
  5. filtrationwas collected by filtration
  6. washwashed with ethyl acetate 10
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-cb31bb7f5900478c8ebe2f3eca5bbab7
Quelldatensatz
uspto-grants-1998_02
Patentnummer
US05716971

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